CN112701306B - Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof - Google Patents

Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof Download PDF

Info

Publication number
CN112701306B
CN112701306B CN202110131216.1A CN202110131216A CN112701306B CN 112701306 B CN112701306 B CN 112701306B CN 202110131216 A CN202110131216 A CN 202110131216A CN 112701306 B CN112701306 B CN 112701306B
Authority
CN
China
Prior art keywords
nickel
carbon film
electrode
electrodeposition
film
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.)
Active
Application number
CN202110131216.1A
Other languages
Chinese (zh)
Other versions
CN112701306A (en
Inventor
尹艳红
文敏
吴子平
黎业生
刘先斌
邓朋
张克
湛钦淇
高文静
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.)
Jiangxi University of Science and Technology
Original Assignee
Jiangxi 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 Jiangxi University of Science and Technology filed Critical Jiangxi University of Science and Technology
Priority to CN202110131216.1A priority Critical patent/CN112701306B/en
Publication of CN112701306A publication Critical patent/CN112701306A/en
Application granted granted Critical
Publication of CN112701306B publication Critical patent/CN112701306B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9041—Metals or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • 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
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • 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
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8803—Supports for the deposition of the catalytic active composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8817—Treatment of supports before application of the catalytic active composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • H01M4/8853—Electrodeposition
    • 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
    • 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
    • Y02E60/50—Fuel cells

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Electrochemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Cell Electrode Carriers And Collectors (AREA)

Abstract

A nickel iron/carbon film-nickel integrated composite electrode and a preparation method thereof belong to the technical field of nano catalytic electrodes. The invention successfully prepares an integrated composite electrode (nickel iron/carbon film-nickel) consisting of a nickel iron and nickel modified carbon nanotube film by utilizing an electrodeposition technology. The introduction of the nickel particles greatly improves the hydrophilicity and the conductivity of the surface of the carbon nano tube film, further induces the uniform distribution of the nickel-iron nano particles on the surface of the carbon nano tube bundle, and the obtained nickel-iron/carbon film-nickel integrated composite electrode has excellent oxygen evolution performance and stability. The nickel-iron/carbon film-nickel integrated composite electrode has the advantages of flexibility, light weight, no adhesive and the like, and can be widely applied to the relevant electrochemical fields of portable energy storage and conversion devices and the like.

Description

Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof
Technical Field
The invention belongs to the field of nano catalytic electrode materials, and particularly relates to a preparation method of a nickel iron/carbon film-nickel integrated composite electrode.
Background
Conventional methods for preparing electrode materials generally employ polymeric binders (e.g., perfluorosulfonic acid (Nafion), Polytetrafluoroethylene (PTFE)) to bind the catalytically active material to the conductive substrate. However, the polymer binder inevitably reduces the intrinsic activity and durability of the catalyst, mainly due to the large contact resistance of the binder, which is easily desorbed during electrocatalysis. To date, some new studies have found that anchoring catalytically active species onto a conductive substrate (e.g., metal foam, metal foil, carbon-based nanomaterials) by in situ growth can directly serve as an integrated electrode without the need for additional polymeric binders. However, the catalytic active material supported by conventional conductive substrates (e.g., nickel foam, nickel foil, nickel mesh) is bulky and difficult to withstand folding or bending, which severely hinders their use in portable devices.
Currently, binderless integrated electrodes are typically designed using a flexible, lightweight carbon-based substrate on which catalytically active species are grown for direct application to portable devices for energy conversion and storage. However, the carbon substrate is not highly hydrophilic in an aqueous solution, which is disadvantageous for growing metal catalyst particles on its surface by a liquid phase method. How to in-situ grow the metal nano-catalyst with uniform particles on the surface of the carbon substrate by surface modification still needs to be deeply researched.
Disclosure of Invention
The invention aims to provide a nickel iron/carbon film-nickel integrated composite electrode. Specifically, nickel particles are introduced into one surface of the carbon nanotube film to modify the surface of the carbon nanotube film. And then introducing nickel-iron particles on the other surface of the carbon film to prepare the sandwich structure flexible integrated composite electrode.
The invention also aims to provide a preparation method of the nickel iron/carbon film-nickel integrated composite electrode.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a nickel iron/carbon film-nickel integrated composite electrode sequentially comprises the following steps
(1) Prepared by vapor deposition to have a certain thickness (0.1-1 μm) and area (1-5 cm)2) The carbon film of (3);
(2) preparing an electroplating solution: 150-350 g L-1Nickel sulfate, 40-60 g L-1Sulfuric acid, 60-80 g L-1Nickel chloride, 1-3 g L-1Sodium lauryl sulfate;
(3) preparing a carbon film-nickel composite film by an electroplating method: adopting a direct current power supply to carry out electrodeposition of metallic nickel on one side of the carbon film, connecting the negative electrode of the power supply with the carbon film, connecting the positive electrode of the power supply with a nickel plate, wherein the electroplating voltage is 2-5V, and the electroplating current is 1-3A dm-2The plating time is 10-50 s. The contact area of the negative carbon film and the electrolyte is 0.2 mA cm-2；
(4) Preparing an electrodeposition solution: 1-3 g L-1Nickel sulfate, 1-3 g L-1Iron sulfate 2-5 g L-1Ammonium sulfate in 0.5 mol L-1Regulating the pH value of the solution to 3-5 by using sulfuric acid;
(5) preparing a nickel iron/carbon film-nickel integrated electrode by electrodeposition: electrodeposition was carried out in a three-electrode system of an electrochemical workstation. The counter electrode is a platinum sheet electrode, the reference electrode is a saturated calomel electrode, and the working electrode is a carbon film-nickel. The voltage of the electro-deposition is-1.5V-1.9V, and the time of the electro-deposition is 300-500 s.
The nickel-iron/carbon film-nickel integrated composite electrode provided by the invention has a self-supporting effect, does not need to use a polymerization adhesive, can be directly used as a catalytic electrode, and simplifies the process steps. The introduction of nickel particles greatly improves the hydrophilicity and the conductivity of the carbon film, and further induces the nickel-iron nano particle layer to be uniformly dispersed on the surface of the carbon nanotube bundle in the carbon film. The sandwich structure design effectively improves the electrochemical performance and stability of the active substance. The carbon nanotube film has the characteristics of light weight, flexibility and the like, and is beneficial to realizing the application of the carbon nanotube film in portable equipment.
The invention has the following beneficial effects: the nickel-iron bimetallic particles grow on the surface of the carbon nano tube film modified by nickel by adopting electroplating and electrodeposition synthesis technology and taking the nickel-modified carbon nano tube film as a substrate. The nickel-modified carbon film has better hydrophilicity and higher conductivity, so that the nickel-iron bimetallic particles are easier to anchor on the surface of the carbon film and grow along the carbon nanotube bundles. The nickel-modified nickel-iron/carbon film integrated composite electrode has the advantages of flexibility, light weight, no binder, simple preparation process and the like, is suitable for batch production, and can be applied to portable electrochemical fields such as water electrolysis, fuel cells and the like.
Drawings
FIG. 1 is a scanning electron microscope image of the Ni-Fe/carbon film integrated composite electrode (NiFe/CMF) in example 1.
FIG. 2 is the SEM image of the Ni-Fe/C film-Ni integrated composite electrode (NiFe/CMF-Ni) in example 2.
Fig. 3 is a comparison of the hydrophilicity and conductivity of the samples of example 1 and example 2.
FIG. 4 is a comparison of the stability of the nickel-iron/carbon film integrated composite electrode (NiFe/CMF) of example 1 and the nickel-iron/carbon film-nickel integrated composite electrode (NiFe/CMF-Ni) of example 2.
FIG. 5 is a flexibility display diagram of the nickel-iron/carbon film-nickel integrated composite electrode (NiFe/CMF-Ni) in example 2.
Detailed Description
The following are specific embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the scope of the present invention is not limited to the following examples. In addition, the technical features involved in the respective embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1.
(1) Prepared by vapor deposition to have a thickness (0.5 μm) and area (4 cm)-2) The carbon film of (1).
(2) Depositing on one side of the carbon film by electrodepositionAnd (4) depositing a ferronickel bimetal. Preparing an electrodeposition solution: 2.1 g L-1Nickel sulfate, 2.2 g L-1Iron sulfate, 3.3 g L-1Ammonium sulfate in 0.5 mol L-1Sulfuric acid adjusted the solution pH to 4. Electrodeposition was carried out in a three-electrode system of an electrochemical workstation. The platinum sheet electrode is used as a counter electrode, the saturated calomel electrode is used as a reference electrode, and the carbon film is used as a working electrode. The electrodeposition voltage was-1.7V and the electrodeposition time was 400 s. And taking out the composite film, and drying to obtain the nickel-iron/carbon film integrated composite electrode (NiFe/CMF). (this material was used as a comparative sample)
Example 2.
(1) Prepared by vapor deposition to have a certain thickness (0.5 μm) and area (3 cm)-2) The carbon film of (1).
(2) And electrodepositing metallic nickel on one surface of the carbon film by adopting an electroplating method. Preparing an electroplating solution: 270 g L-1Nickel sulfate, 50 g L-1Sulfuric acid, 70 g L-1Nickel chloride, 2 g L-1 C12H25NaO4And S. The contact area of the carbon film and the electrolyte is 0.2 mA cm-2. The negative electrode of the power supply is connected with the carbon film, the positive electrode is connected with the nickel plate, the voltage is 3V, and the current is 2A dm-2The plating time was 10 seconds. Taking out the carbon film-nickel composite film and drying. (3) And depositing ferronickel bimetal on the other surface of the carbon film-nickel composite film by an electrodeposition method. Preparing an electrodeposition solution: 2.1 g L-1Nickel sulfate, 2.2 g L-1Iron sulfate, 3.3 g L-1Ammonium sulfate in 0.5 mol L-1Sulfuric acid adjusted the solution pH to 4. Electrodeposition was carried out in a three-electrode system of an electrochemical workstation. The platinum sheet electrode is used as a counter electrode, the saturated calomel electrode is used as a reference electrode, and the carbon film-nickel composite film is used as a working electrode. The electrodeposition voltage was-1.7V and the electrodeposition time was 400 s. Taking out the composite film, and drying to obtain the nickel iron/carbon film-nickel integrated composite electrode (NiFe/CMF-Ni).
Example 3.
(1) Prepared by vapor deposition to have a certain thickness (0.2 μm) and area (2 cm)-2) The carbon film of (1).
(2) By electroplatingAnd electrodepositing metallic nickel on one surface of the carbon film. Preparing an electroplating solution: 270 g L-1Nickel sulfate, 50 g L-1Sulfuric acid, 70 g L-1Nickel chloride, 2 g L-1 C12H25NaO4And S. The contact area of the carbon film and the electrolyte is 0.2 mA cm-2. The negative electrode of the power supply is connected with the carbon film, the positive electrode is connected with the nickel plate, the voltage is 3V, and the current is 2A dm-2The plating time was 20 s. Taking out the carbon film-nickel composite film and drying. (3) And depositing ferronickel bimetal on the other surface of the carbon film-nickel composite film by an electrodeposition method. Preparing an electrodeposition solution: 2.1 g L-1Nickel sulfate, 2.2 g L-1Iron sulfate, 3.3 g L-1Ammonium sulfate in 0.5 mol L-1Sulfuric acid adjusted the solution pH to 4. Electrodeposition was carried out in a three-electrode system of an electrochemical workstation. The platinum sheet electrode is used as a counter electrode, the saturated calomel electrode is used as a reference electrode, and the carbon film-nickel composite film is used as a working electrode. The electrodeposition voltage was-1.7V and the electrodeposition time was 300 s. Taking out the composite film, and drying to obtain the nickel iron/carbon film-nickel integrated composite electrode (NiFe/CMF-Ni).
Example 4.
(1) Prepared by vapor deposition to have a certain thickness (0.3 μm) and area (3 cm)-2) The carbon film of (1).
(2) And electrodepositing metallic nickel on one surface of the carbon film by adopting an electroplating method. Preparing an electroplating solution: 270 g L-1Nickel sulfate, 50 g L-1Sulfuric acid, 70 g L-1Nickel chloride, 2 g L-1 C12H25NaO4And S. The contact area of the carbon film and the electrolyte is 0.2 mA cm-2. The negative electrode of the power supply is connected with the carbon film, the positive electrode is connected with the nickel plate, the voltage is 3V, and the current is 2A dm-2The plating time was 30 s. Taking out the carbon film-nickel composite film and drying. (3) And depositing ferronickel bimetal on the other surface of the carbon film-nickel composite film by an electrodeposition method. Preparing an electrodeposition solution: 2.1 g L-1Nickel sulfate, 2.2 g L-1Iron sulfate, 3.3 g L-1Ammonium sulfate in 0.5 mol L-1Sulfuric acid adjusted the solution pH to 4. Electrodeposition was carried out in a three-electrode system of an electrochemical workstation. Platinum sheet electrode as counter electrode, saturatedThe calomel electrode is used as a reference electrode, and the carbon film-nickel composite film is used as a working electrode. The electrodeposition voltage was-1.7V and the electrodeposition time was 500 s. Taking out the composite film, and drying to obtain the nickel iron/carbon film-nickel integrated composite electrode (NiFe/CMF-Ni).
Example 5.
(1) Prepared by vapor deposition to have a thickness (0.5 μm) and area (4 cm)-2) The carbon film of (1).
(2) And electrodepositing metallic nickel on one surface of the carbon film by adopting an electroplating method. Preparing an electroplating solution: 270 g L-1Nickel sulfate, 50 g L-1Sulfuric acid, 70 g L-1Nickel chloride, 2 g L-1 C12H25NaO4And S. The contact area of the carbon film and the electrolyte is 0.2 mA cm-2. The negative electrode of the power supply is connected with the carbon film, the positive electrode is connected with the nickel plate, the voltage is 3V, and the current is 2A dm-2The plating time was 40 s. Taking out the carbon film-nickel composite film and drying. (3) And depositing ferronickel bimetal on the other surface of the carbon film-nickel composite film by an electrodeposition method. Preparing an electrodeposition solution: 2.1 g L-1Nickel sulfate, 2.2 g L-1Iron sulfate, 3.3 g L-1Ammonium sulfate in 0.5 mol L-1Sulfuric acid adjusted the solution pH to 4. Electrodeposition was carried out in a three-electrode system of an electrochemical workstation. The platinum sheet electrode is used as a counter electrode, the saturated calomel electrode is used as a reference electrode, and the carbon film-nickel composite film is used as a working electrode. The electrodeposition voltage was-1.7V and the electrodeposition time was 300 s. Taking out the composite film, and drying to obtain the nickel iron/carbon film-nickel integrated composite electrode (NiFe/CMF-Ni).

Claims (2)

1. The nickel-iron/carbon film-nickel integrated composite electrode is characterized by being prepared by a preparation method sequentially comprising the following steps of:
(1) preparing a carbon film by adopting a vapor deposition method; the carbon film has a thickness of 0.1-1 μm and an area of 1-5 cm2(ii) a The carbon film is a carbon nanotube film;
(2) preparing an electroplating solution: 150-350 g L-1Nickel sulfate, 40-60 g L-1Sulfuric acid, 60-80 g L-1Nickel chloride, 1-3 g L-1Sodium lauryl sulfate;
(3) preparing a carbon film-nickel composite film by an electroplating method: adopting a direct current power supply to carry out electrodeposition of metallic nickel on one side of the carbon film, connecting the negative electrode of the power supply with the carbon film, connecting the positive electrode of the power supply with a nickel plate, wherein the electroplating voltage is 2-5V, and the electroplating current is 1-3A dm-2The electroplating time is 10-50 s; the contact area of the negative carbon film and the plating solution is 0.2 mA cm-2(ii) a The electroplating solution is the electroplating solution prepared in the step (2);
(4) preparing an electrodeposition solution: 1-3 g L-1Nickel sulfate, 1-3 g L-1Iron sulfate 2-5 g L-1Ammonium sulfate in 0.5 mol L-1Regulating the pH value of the solution to 3-5 by using sulfuric acid;
(5) and (3) performing electrodeposition on the other surface of the carbon film-nickel composite film obtained in the step (3) on which the metal nickel is not electrodeposited to prepare a nickel iron/carbon film-nickel integrated electrode: carrying out electrodeposition in a three-electrode system of an electrochemical workstation; the counter electrode is a platinum sheet electrode, the reference electrode is a saturated calomel electrode, and the working electrode is a carbon film-nickel; the voltage of the electrodeposition is-1.5V-1.9V, and the time of the electrodeposition is 300-500 s; the electrodeposition solution is the electrodeposition solution prepared in the step (4).
2. A preparation method of a nickel iron/carbon film-nickel integrated composite electrode is characterized by sequentially comprising the following steps of:
(1) preparing a carbon film by adopting a vapor deposition method; the carbon film has a thickness of 0.1-1 μm and an area of 1-5 cm2(ii) a The carbon film is a carbon nanotube film;
(2) preparing an electroplating solution: 150-350 g L-1Nickel sulfate, 40-60 g L-1Sulfuric acid, 60-80 g L-1Nickel chloride, 1-3 g L-1Sodium lauryl sulfate;
(3) preparing a carbon film-nickel composite film by an electroplating method: adopting a direct current power supply to carry out electrodeposition of metallic nickel on one side of the carbon film, connecting the negative electrode of the power supply with the carbon film, connecting the positive electrode of the power supply with a nickel plate, wherein the electroplating voltage is 2-5V, and the electroplating current is 1-3A dm-2The electroplating time is 10-50 s; the contact area of the negative carbon film and the plating solution was 0.2mA cm-2(ii) a The electroplating solution is the electroplating solution prepared in the step (2);
(4) preparing an electrodeposition solution: 1-3 g L-1Nickel sulfate, 1-3 g L-1Iron sulfate 2-5 g L-1Ammonium sulfate in 0.5 mol L-1Regulating the pH value of the solution to 3-5 by using sulfuric acid;
(5) and (3) performing electrodeposition on the other surface of the carbon film-nickel composite film obtained in the step (3) on which the metal nickel is not electrodeposited to prepare a nickel iron/carbon film-nickel integrated electrode: carrying out electrodeposition in a three-electrode system of an electrochemical workstation; the counter electrode is a platinum sheet electrode, the reference electrode is a saturated calomel electrode, and the working electrode is a carbon film-nickel; the voltage of the electrodeposition is-1.5V-1.9V, and the time of the electrodeposition is 300-500 s; the electrodeposition solution is the electrodeposition solution prepared in the step (4).
CN202110131216.1A 2021-01-30 2021-01-30 Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof Active CN112701306B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110131216.1A CN112701306B (en) 2021-01-30 2021-01-30 Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110131216.1A CN112701306B (en) 2021-01-30 2021-01-30 Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof

Publications (2)

Publication Number Publication Date
CN112701306A CN112701306A (en) 2021-04-23
CN112701306B true CN112701306B (en) 2022-03-22

Family

ID=75516497

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110131216.1A Active CN112701306B (en) 2021-01-30 2021-01-30 Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof

Country Status (1)

Country Link
CN (1) CN112701306B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114351198A (en) * 2022-01-13 2022-04-15 常州大学 Preparation method of extensible nickel-containing carbon nanotube-copper composite film

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1544707A (en) * 2003-11-13 2004-11-10 上海交通大学 Process for preparing nickel-based nano-tube composite material by composite electrodeposition
CN110947387A (en) * 2019-11-25 2020-04-03 中国工程物理研究院材料研究所 Preparation method and application of nickel-iron double metal hydroxide nano film material
CN111910225A (en) * 2020-06-22 2020-11-10 西安交通大学 Method for simultaneously depositing nickel-iron modified titanium dioxide nanotube electrode

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101457357A (en) * 2007-12-14 2009-06-17 比亚迪股份有限公司 Film coating material and preparation method thereof
CN101255591B (en) * 2008-04-03 2011-01-26 厦门大学 Method for preparing carbon nano-tube/nano-nickel composite film
CN103400703A (en) * 2013-07-12 2013-11-20 天津大学 Self-supporting CNT (Carbon Nano-Tube) film-faradaic pseudocapacitance composite material
CN108193227A (en) * 2016-12-08 2018-06-22 中国科学院大连化学物理研究所 Oxygen electrode and its preparation and application are analysed in the electro-catalysis of nickel-ferric spinel base
CN107541758A (en) * 2017-08-01 2018-01-05 昆明理工大学 A kind of method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating
CN109136986B (en) * 2018-10-29 2020-05-22 高彪峰 Preparation method of nano nickel/array carbon nanotube composite material
CN110528022B (en) * 2019-08-13 2021-04-20 中国工程物理研究院材料研究所 Preparation method of nitrogen-doped carbon nano array-nickel iron hydrotalcite oxygen evolution electrode
CN111905744B (en) * 2020-07-23 2022-09-09 安徽工业大学 Nickel-iron hydroxide composite material, catalyst, preparation method and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1544707A (en) * 2003-11-13 2004-11-10 上海交通大学 Process for preparing nickel-based nano-tube composite material by composite electrodeposition
CN110947387A (en) * 2019-11-25 2020-04-03 中国工程物理研究院材料研究所 Preparation method and application of nickel-iron double metal hydroxide nano film material
CN111910225A (en) * 2020-06-22 2020-11-10 西安交通大学 Method for simultaneously depositing nickel-iron modified titanium dioxide nanotube electrode

Also Published As

Publication number Publication date
CN112701306A (en) 2021-04-23

Similar Documents

Publication Publication Date Title
Li et al. Hybridizing NiCo2O4 and Amorphous Ni x Co y Layered Double Hydroxides with Remarkably Improved Activity toward Efficient Overall Water Splitting
Döner et al. Effect of C-felt supported Ni, Co and NiCo catalysts to produce hydrogen
CN106669739A (en) Transition metal sulfide/carbon nanotube composite material as well as preparation method and application thereof
Feng et al. Ni–Zn nanosheet anchored on rGO as bifunctional electrocatalyst for efficient alkaline water-to-hydrogen conversion via hydrazine electrolysis
CN110205636A (en) A kind of preparation method of self-cradling type three-dimensional porous structure double-function catalyzing electrode
CN109837558A (en) A kind of preparation method of the FeOOH that hydrothermal electrodeposition combines-nickel-ferric spinel analysis oxygen electrode
CN110433829B (en) MoO (MoO)2-NiSx/CC hydrogen evolution electrocatalyst and preparation method thereof
Yang et al. Electrocatalytic properties of porous Ni-Co-WC composite electrode toward hydrogen evolution reaction in acid medium
CN112481656B (en) Bifunctional catalyst for high-selectivity electrocatalysis of glycerin oxidation conversion to produce formic acid and high-efficiency electrolysis of water to produce hydrogen, preparation method and application thereof
CN106207091A (en) A kind of lithium ion battery flexibility positive pole, its preparation method and the super full battery of flexible lithium ion
CN113529120A (en) Transition metal sulfide composite electrode, preparation method and application thereof
CN112701306B (en) Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof
CN108075142B (en) Preparation method of nano-array catalyst layer for anion exchange membrane fuel cell
CN113957480B (en) Copper-based catalyst for electrochemical catalysis of carbon dioxide reduction and energy storage, electrode, preparation method and application thereof
Wang et al. Hierarchical flower-like amorphous nickel sulfide/crystalline CoFe layered double hydroxide heterostructure for overall water splitting
CN108273524B (en) Carbon composite material modified by chalcogenide and transition metal and preparation method and application thereof
CN106449141B (en) Ti-alloy mesh substrate based on highly conductive ceramic watch facial mask prepares cobalt hydroxide/nickel electrode of super capacitor method
CN108538645A (en) A kind of preparation method of carbon/transition metal based combined electrode and products thereof and purposes
CN116024583A (en) Nickel sulfide nano rod array electrocatalytic material and preparation method and application thereof
CN110129814B (en) Electrocatalytic electrode with ditungsten carbide inverse opal composite micro-nano structure and preparation and hydrogen evolution application thereof
CN109599564B (en) Nickel cobaltate array self-supporting large-area air electrode and preparation and application thereof
Wei et al. Rapid preparation of high-efficiency hydrogen evolution catalysts with decent hydrophilicity on cheap carbon steel
CN111020627B (en) Method for chemically plating NiP on surface of multi-wall carbon nano tube
CN115323393B (en) Method for preparing nickel-based bimetallic hydrogen evolution catalyst by anodic dissolution electrodeposition in eutectic ionic liquid
WO2023082414A1 (en) Carbon dioxide energy storage system driven by new energy and electric energy, and energy storage method

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
GR01 Patent grant
GR01 Patent grant