CN113846344A - Nickel disulfide oxygen evolution catalyst rich in edge active sites and preparation method thereof - Google Patents

Nickel disulfide oxygen evolution catalyst rich in edge active sites and preparation method thereof Download PDF

Info

Publication number
CN113846344A
CN113846344A CN202111304598.XA CN202111304598A CN113846344A CN 113846344 A CN113846344 A CN 113846344A CN 202111304598 A CN202111304598 A CN 202111304598A CN 113846344 A CN113846344 A CN 113846344A
Authority
CN
China
Prior art keywords
nickel
oxygen evolution
reaction
active sites
drying
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
CN202111304598.XA
Other languages
Chinese (zh)
Inventor
闫卿
孔丽
高瑞芹
陈正飞
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.)
Zhejiang University of Science and Technology ZUST
Original Assignee
Zhejiang University of Science and Technology ZUST
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 Zhejiang University of Science and Technology ZUST filed Critical Zhejiang University of Science and Technology ZUST
Priority to CN202111304598.XA priority Critical patent/CN113846344A/en
Publication of CN113846344A publication Critical patent/CN113846344A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
    • C25B1/02Hydrogen or oxygen
    • C25B1/04Hydrogen or oxygen by electrolysis of water
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C25B11/03Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
    • C25B11/031Porous electrodes
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/054Electrodes comprising electrocatalysts supported on a carrier
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention discloses a novel nickel disulfide oxygen evolution catalyst rich in edge active sites and a preparation method thereof, wherein the method comprises the following steps: mixing nickel salt and NH4NO3Dissolving in distilled water, and dropwise adding ammonia water under stirring to form a uniform solution; pretreating the foamed nickel, then placing the pretreated foamed nickel into a uniform solution, and carrying out a closed reaction to obtain a foamed nickel-loaded nickel hydroxide precursor; washing and drying the nickel foam loaded nickel hydroxide precursor, and then calcining to obtain NiO/NF; mixing Na2S·9H2Dissolving O in water, adding NiO/NF to react, washing and drying the product after reaction to obtain the product rich in fringingNickel disulfide oxygen evolution catalyst of the sex site. The invention is based on cheap transition metal nickel salt, and prepares Ni rich in edge active sites by adopting a simple and repeatable ammonia water complex deposition method and a sintering method3S2the/NF electrode is used for catalyzing oxygen evolution reaction.

Description

Nickel disulfide oxygen evolution catalyst rich in edge active sites and preparation method thereof
Technical Field
The invention relates to the technical field of nickel disulfide oxygen evolution catalysts, in particular to a novel nickel disulfide oxygen evolution catalyst rich in edge active sites and a preparation method thereof.
Background
Hydrogen production by water electrolysis is one of the key core technologies of renewable resources in the task of finding clean energy sources for replacing fossil fuel energy sources. The greatest disadvantage of electrochemical cells for water splitting is due to the high overpotential of the existing water oxidation catalysts required for the anode. Ruthenium (Ru) and iridium (Ir) based catalysts are the most efficient Oxygen Evolution Reaction (OER) electrocatalysts, but they are scarce, expensive and the limited supply of these noble metal based electrocatalysts is not sufficient for industrial water decomposition. Therefore, highly active, earth-rich, and durable oxygen evolution catalysts were developed.
Rich source, low cost, and environment-friendly transition metal sulfide (such as NiS)2、FeS2/CoS2、Ni3S2、Co-MoS2Etc.) have been reported as promising OER electrocatalysts. More recently, nickel sulfides, especially Ni3S2The phases, due to their high electrical conductivity and good electrocatalytic properties, are attractive electrocatalysts. For example, (003) -face exposed Ni synthesized by Dong et al via anodic oxidation and steam sulfidation strategies3S2The nano porous film has a driving current density of 20mA cm-2The overpotential is 319 mV. However, the performance of the latest electrocatalysts still does not meet the requirements of industrial manufacture. The large number of active sites may further improve the catalytic performance of the electrocatalyst. For Ni with more active sites3S2It is a good strategy to create many edges and defects for the catalyst. In addition, electrode structure should be considered in adjusting electrocatalytic activity and stability to OER. Powdered electrocatalysts typically require the addition of a polymeric binder (e.g., Nafion) to prepare the final electrode. Traditional cast fabrication techniques may destroy the unique micro-nano structure of the catalyst, inevitably reducing exposed active sites and hindering the release of diffusing electrolyte ions and oxygen bubbles. Thus, in situ bonding directly on a conductive substrateRich edge Ni3S2Electrocatalysts are a viable means of achieving high efficiency electrocatalytic activity and oxygen evolution reaction durability. Furthermore, the oxygen evolution reaction is a complex reaction with four successive proton-coupled electron transfer steps, and Ni3S2Are thermodynamically less stable than metal oxides. Therefore, finding the actual active substance is an important task.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a self-supporting trinickel disulfide oxygen evolution catalyst rich in edge active sites and a preparation method thereof, the catalyst is attached to a current collector without extra stirring for sample preparation, and meanwhile, the catalyst has rich active sites and can ensure that an electrode can be ensured to be under a larger current density (100mA cm)-2) High-efficiency and stable service.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, a preparation method of a nickel disulfide oxygen evolution catalyst rich in edge active sites is provided, which comprises the following steps:
(1) mixing nickel salt and NH4NO3Dissolving in distilled water, and dropwise adding ammonia water under stirring to form a uniform solution;
(2) pretreating the foamed nickel, then immersing the pretreated foamed nickel into the uniform solution prepared in the step (1), and carrying out a closed reaction to obtain a foamed nickel-loaded nickel hydroxide precursor;
(3) washing and drying the precursor of the nickel hydroxide loaded on the foamed nickel prepared in the step (2), and then calcining to obtain NiO/NF, namely nickel oxide loaded on the foamed nickel;
(4) mixing Na2S·9H2Dissolving O in water, adding the NiO/NF prepared in the step (3), heating for reaction, washing and drying a product after the reaction to obtain Ni3S2/NF, i.e., a nickel disulfide oxygen evolution catalyst rich in edge active sites.
Preferably, in step (1), the nickel salt is reacted with NH4NO3The molar ratio of (A) to (B) is 2: 1; the nickel salt is selected from NiSO4·6H2O、Ni(NO3)2、Ni(CH3COO)2Or NiCl2
Preferably, the dropping speed of the ammonia water is 1 drop/s; the concentration of ammonia water contained in the homogeneous solution was 10 wt%.
Preferably, in step (2), the pretreatment is: washing the foamed nickel for 15-40 min by using dilute hydrochloric acid, acetone and deionized water in sequence respectively; the concentration of the dilute hydrochloric acid is 6M.
Preferably, in the step (2), the temperature of the sealing reaction is 90 ℃ and the time is 6-24 h.
Preferably, in the step (3), deionized water and absolute ethyl alcohol are used for washing in sequence; the temperature of the drying was 60 ℃.
Preferably, in step (3), the calcination is: at 5 deg.C for min in air atmosphere-1The temperature rising rate of (2) is calcined at 350 ℃ for 2 h.
Preferably, in the step (4), the Na is2S·9H2The molar ratio of O to nickel salt is more than 1: 1; na (Na)2S·9H2O is dissolved in water to a concentration of 1 to 10 mM.
Preferably, in the step (4), the reaction temperature is 160 ℃, and the reaction time is 8 h; the drying temperature is 60 ℃, and the drying time is 6-24 hours.
In a second aspect of the invention, the nickelic disulfide oxygen evolution catalyst rich in edge active sites prepared by the preparation method is provided.
In a third aspect of the invention, the application of the nickel disulfide oxygen evolution catalyst rich in edge active sites in catalyzing oxygen evolution reaction is provided.
The invention has the beneficial effects that:
(1) the invention is based on cheap transition metal nickel salt, and prepares Ni rich in edge active sites by adopting a simple and repeatable ammonia water complex deposition method and a sintering method3S2the/NF electrode is used for catalyzing oxygen evolution reaction.
(2) The invention converts two-dimensional Ni3S2The nano-sheet grows in situ on the three-dimensional conductive foam nickel matrix to be used as a self-supporting electrode, so that the use of a high-molecular binder can be avoided, and the electrode material can be reinforcedIs used for the electrical conductivity of (1). The micro-nano hierarchical structure with the open 3D can promote electrolyte ion diffusion and oxygen molecule release, avoid failure of active sites and guarantee long-time efficient work of electrode materials.
(3) Ni prepared by the invention3S2The current density of the/NF electrode is 20, 50 and 100 mA-cm-2The next continuous operation for 10 hours can be carried out efficiently and stably, the potential is only increased by 1.5 percent in the whole process, and the electrode Ni is3S2the/NF has good long-term working stability. Illustrating Ni obtained by optimizing the material structure3S2the/NF electrode has the industrial application potential of alkaline electrocatalytic oxygen evolution.
Drawings
FIG. 1 shows Ni prepared in example 33S2Electron scanning pictures of/NF electrodes.
FIG. 2 shows Ni prepared in example 33S2High resolution transmission HRTEM image of/NF.
FIG. 3 shows Ni prepared in example 33S2NF in alkaline environment, 100mA cm-2Chronopotentiometric curve below.
FIG. 4 is an X-ray diffraction (XRD) pattern of NiO/NF prepared in comparative example.
FIG. 5 is a scanning picture of NiO/NF prepared by comparative example.
FIG. 6 shows Ni prepared in example 33S2XRD pattern of/NF.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background section, Ni is already present3S2The performance of the phase electrocatalyst still cannot meet the requirements of industrial manufacture, and the active sites need to be added to further improve the catalytic performance of the electrocatalyst.
Based on the above, the object of the present invention is to provide a self-supporting di-compound rich in edge active sitesA nickel sulfide oxygen evolution catalyst and a preparation method thereof. The invention designs the foam nickel loaded Ni with rich edges by adopting simple two-step electrolytic oxygen evolution3S2And an electrode. Open nanostructure Ni with abundant nanopores3S2Mass transfer of the electrolyte and release of oxygen molecules can be promoted. In addition, the large number of active edges provides more active sites, further promoting Ni3S2OER procedure above. In addition, the present inventors also investigated Ni after a 10-hour chronopotentiometric excitation test3S2And an electrode. Research shows that the Ni prepared by the invention3S2The actual composition of the catalyst is Ni3S2-a NiOOH heterojunction structure. Ni as precatalyst3S2Exhibits high electrochemical activity for OER under alkaline conditions. Furthermore, OER performance can be at 100mA cm-2Is stable at high current densities.
Ni prepared by the invention3S2The generation of rich edge active sites in the catalyst is: placing a precursor of the nickel hydroxide loaded on the foam nickel in a muffle furnace for calcination, wherein the absence of water molecules causes a porous defect to be generated among the generated nickel oxide crystals, and the defect is concentrated on the edge of a crystal face; defects are retained during further sulfidisation, thereby giving the sulfide an edge active site.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and commercially available.
Example 1:
synthesizing nickel disulfide by taking nickel nitrate as a nickel source:
(1)Ni(NO3)2and NH4NO3Weighing according to the mol ratio of 2: 1, dissolving the mixture in distilled water, and then dropwise adding ammonia water under the stirring state to form a uniform solution A;
(2) pretreating foamed nickel, and sequentially washing with 6M dilute hydrochloric acid, acetone and deionized water for 15 min. Immersing the pretreated foamed nickel into the uniform solution A prepared in the step (2), transferring the solution and the pretreated foamed nickel into a culture dish with a cover, and keeping the solution and the pretreated foamed nickel at 90 ℃ for 12 hours to obtain the foamed nickel-loaded nickel hydroxide precursor.
(3) Washing the foam nickel-loaded nickel hydroxide precursor prepared in the step (2) by using deionized water and absolute ethyl alcohol in sequence; then dried in an oven at 60 ℃ for 5 h. Then it was put in an air atmosphere at 5 ℃ for min-1The nickel oxide supported on the foamed nickel (NiO/NF) is obtained by calcining the nickel oxide at 350 ℃ for 2h in a muffle furnace.
(4) According to Na2S·9H2O and Ni (NO)3)2In a molar ratio of 2: 1, weighing Na2S·9H2O, mixing with Na2S·9H2O was dissolved in water to a concentration of 5mM, and the solution and the above NiO/NF were transferred to a polytetrafluoroethylene-lined stainless steel autoclave (volume 45mL) and heated at 160 ℃ for 8 hours. Taking out the product after the reaction is finished, washing the product with deionized water, and then drying the product in an oven at 60 ℃ for 6 hours to obtain Ni rich in edge active sites3S2/NF。
Example 2:
synthesizing nickel disulfide by taking nickel chloride as a nickel source:
(1)NiCl2and NH4NO3Weighing according to the molar ratio of 2: 1, dissolving in distilled water, and dropwise adding ammonia water under stirring to form a uniform solution A.
(2) Pretreating foamed nickel, and sequentially washing with 6M dilute hydrochloric acid, acetone and deionized water for 15 min. Immersing the pretreated foamed nickel into the uniform solution A prepared in the step (2), transferring the solution and the pretreated foamed nickel into a culture dish with a cover, and keeping the solution and the pretreated foamed nickel at 90 ℃ for 12 hours to obtain the foamed nickel-loaded nickel hydroxide precursor.
(3) Washing the foam nickel-loaded nickel hydroxide precursor prepared in the step (2) by using deionized water and absolute ethyl alcohol in sequence; then dried in an oven at 60 ℃ for 6 h. Then it was put in an air atmosphere at 5 ℃ min-1The temperature rise rate of the nickel oxide is calcined in a muffle furnace at 350 ℃ for 2h to obtain the nickel oxide (NiO/NF) loaded on the foamed nickel.
(4) According to Na2S·9H2O and NiCl2Is referred to as 2: 1, weighing Na2S·9H2O, mixing with Na2S·9H2O was dissolved in water to a concentration of 5mM and dissolved in 32mL of H2O, the solution and the NiO/NF were then transferred to a polytetrafluoroethylene-lined stainless steel autoclave (volume 45mL) and heated at 160 ℃ for 8 hours. Taking out the product after the reaction is finished, washing the product with deionized water, and then drying the product in an oven at 60 ℃ for 6 hours to obtain Ni rich in edge active sites3S2/NF。
Example 3
(1)NiSO4·6H2O and NH4NO3Weighing according to the molar ratio of 2: 1, dissolving in distilled water, and dropwise adding ammonia water under stirring to form a uniform solution A.
(2) Pretreating the foamed nickel, washing the foamed nickel for 15 minutes by using dilute hydrochloric acid, acetone and deionized water in sequence, then immersing the pretreated foamed nickel into the solution A, transferring the solution and the pretreated foamed nickel into a culture dish with a cover, and keeping the solution and the pretreated foamed nickel for 12 hours at 90 ℃ to obtain the foamed nickel-loaded nickel hydroxide precursor.
(3) Washing the precursor of the nickel hydroxide loaded on the foam nickel by using deionized water and absolute ethyl alcohol, drying for 5 hours in an oven at 60 ℃, and then drying the precursor of the nickel hydroxide loaded on the foam nickel for 5min at 5 ℃ in an air atmosphere-1The nickel oxide is calcined in a muffle furnace for 2 hours at 350 ℃ to obtain the nickel oxide (NiO/NF) loaded on the foamed nickel.
(4) According to Na2S·9H2O and NiCl2In a molar ratio of 2: 1, weighing Na2S·9H2O, mixing with Na2S·9H2O was dissolved in water to a concentration of 5mM, and the solution and the above NiO/NF were transferred to a polytetrafluoroethylene-lined stainless steel autoclave (volume 45mL) and heated at 160 ℃ for 8 hours. Finally, the product Ni is taken out3S2/NF, washing with deionized water several times, and drying in oven at 60 deg.CDrying is carried out for 6 hours.
FIG. 1 shows Ni prepared in example 33S2The electronic scanning picture of the/NF electrode can clearly show that the electrode is in a self-supporting nano sheet network structure. FIG. 2 shows Ni prepared in example 33S2High resolution transmission HRTEM of/NF from which it can be seen that there are abundant active sites at the boundaries of the nanoplate lattice fringes.
Comparative example
(1)NiSO4·6H2O and NH4NO3Weighing according to the molar ratio of 2: 1, dissolving in distilled water, and dropwise adding ammonia water under stirring to form a uniform solution A.
(2) Pretreating the foamed nickel, washing the foamed nickel for 15 minutes by using dilute hydrochloric acid, acetone and deionized water in sequence, then immersing the pretreated foamed nickel into the solution A, transferring the solution and the pretreated foamed nickel into a culture dish with a cover, and keeping the solution and the pretreated foamed nickel for 12 hours at 90 ℃ to obtain the foamed nickel-loaded nickel hydroxide precursor.
(3) Washing the precursor of the nickel hydroxide loaded on the foam nickel by using deionized water and absolute ethyl alcohol, drying for 5 hours in an oven at 60 ℃, and then drying the precursor of the nickel hydroxide loaded on the foam nickel for 5min at 5 ℃ in an air atmosphere-1The temperature rise rate is that the nickel oxide (NiO/NF) loaded on the foamed nickel is obtained after calcining for 2 hours in a muffle furnace at 350 ℃, namely the catalyst.
From FIG. 4, it can be seen that the nano-sheet cross-linked structure of the catalyst NiO/NF is more excellent than that of Ni in example 33S2the/NF (figure 1) is more regular, the surface is smoother, and no Ni exists3S2the/NF is so coarse that the active sites of the catalyst are fewer, and therefore the catalytic performance is better than that of Ni3S2The difference in/NF. FIG. 5 is an XRD pattern of NiO/NF that can demonstrate the successful preparation of NiO/NF, FIG. 6 is Ni3S2XRD of/NF, evidence of Ni3S2Successful preparation of/NF, Ni is seen from XRD diffraction peaks of the two catalysts of FIGS. 5 and 63S2The diffraction peak of/NF was stronger and the peak width was narrower, indicating that the resulting Ni3S2Has higher crystallinity, and is possibly beneficial to improving Ni3S2The intrinsic activity of NF.
Application example
The novel nickel disulfide catalyst rich in edge active sites is applied to electrocatalytic hydrogen evolution: ni prepared in examples 1 to 33S2the/NF electrode and the NiO/NF electrode prepared by the comparative example respectively adopt a standard three-electrode system, and have catalytic effect on the hydrogen evolution reaction process in 1M KOH alkaline solution.
Ni prepared in examples 1 to 33S2The electrocatalytic hydrogen evolution performance of the/NF electrode and the NiO/NF electrode prepared by the comparative example in an alkaline solution is that the current density is 10mA cm-2When the catalyst is used, the three groups of electrodes can ensure that the overpotential is lower than 120 mV; and the electrode NiO/NF overpotential of the comparative example is less than 220 mV.
FIG. 3 shows Ni prepared in example 33S2NF in alkaline environment, 100mA cm-2The chronopotentiometric curve below shows good long-term stability.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (10)

1. A preparation method of a nickel disulfide oxygen evolution catalyst rich in edge active sites is characterized by comprising the following steps:
(1) mixing nickel salt and NH4NO3Dissolving in distilled water, and dropwise adding ammonia water under stirring to form a uniform solution;
(2) pretreating the foamed nickel, then immersing the pretreated foamed nickel into the uniform solution prepared in the step (1), and carrying out a closed reaction to obtain a foamed nickel-loaded nickel hydroxide precursor;
(3) washing and drying the precursor of the nickel hydroxide loaded on the foamed nickel prepared in the step (2), and then calcining to obtain NiO/NF, namely nickel oxide loaded on the foamed nickel;
(4) mixing Na2S·9H2Dissolving O in water, adding the NiO/NF prepared in the step (3), heating for reaction, washing and drying a product after the reaction to obtain Ni3S2/NF, i.e., a nickel disulfide oxygen evolution catalyst rich in edge active sites.
2. The method according to claim 1, wherein in the step (1), the nickel salt is mixed with NH4NO3The molar ratio of (A) to (B) is 2: 1; the nickel salt is selected from NiSO4·6H2O、Ni(NO3)2、Ni(CH3COO)2Or NiCl2
Preferably, the dropping speed of the ammonia water is 1 drop/s; the concentration of ammonia water contained in the homogeneous solution was 10 wt%.
3. The method according to claim 1, wherein in the step (2), the pretreatment is: washing the foamed nickel for 15min by dilute hydrochloric acid, acetone and deionized water in sequence; the concentration of the dilute hydrochloric acid is 6M.
4. The preparation method according to claim 1, wherein in the step (2), the temperature of the sealing reaction is 90 ℃ and the time is 12 hours.
5. The production method according to claim 1, wherein in the step (3), washing is performed using deionized water and anhydrous ethanol in this order; the temperature of the drying was 60 ℃.
6. The method according to claim 1, wherein in the step (3), the calcination is: at 5 deg.C for min in air atmosphere-1The temperature rising rate of (2) is calcined at 350 ℃ for 2 h.
7. The method according to claim 1, wherein in the step (4), the Na is2S·9H2The molar ratio of O to nickel salt is more than 1: 1; na (Na)2S·9H2O is dissolved in water to a concentration of 1 to 10 mM.
8. The preparation method according to claim 1, wherein in the step (4), the reaction temperature is 160 ℃ and the reaction time is 8 h; the drying temperature is 60 ℃, and the drying time is 6-24 hours.
9. The nickel disulfide oxygen evolution catalyst rich in edge active sites prepared by the preparation method of any one of claims 1 to 8.
10. Use of the nickel trinickel disulfide oxygen evolution catalyst rich in edge active sites as defined in claim 9 in catalyzing an oxygen evolution reaction.
CN202111304598.XA 2021-11-05 2021-11-05 Nickel disulfide oxygen evolution catalyst rich in edge active sites and preparation method thereof Pending CN113846344A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111304598.XA CN113846344A (en) 2021-11-05 2021-11-05 Nickel disulfide oxygen evolution catalyst rich in edge active sites and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111304598.XA CN113846344A (en) 2021-11-05 2021-11-05 Nickel disulfide oxygen evolution catalyst rich in edge active sites and preparation method thereof

Publications (1)

Publication Number Publication Date
CN113846344A true CN113846344A (en) 2021-12-28

Family

ID=78984032

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111304598.XA Pending CN113846344A (en) 2021-11-05 2021-11-05 Nickel disulfide oxygen evolution catalyst rich in edge active sites and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113846344A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114990619A (en) * 2022-05-25 2022-09-02 江苏大学 Amorphous NiOOH/Ni 3 S 2 Heterostructure type nickel-based composite catalyst and preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3296431A1 (en) * 2016-09-15 2018-03-21 Ecole Polytechnique Fédérale de Lausanne (EPFL) Method of synthesis of an electrode for use as a catalyst of oxygen evolution reaction
CN110518235A (en) * 2019-07-15 2019-11-29 广东工业大学 A kind of three nickel electrode of self-supporting curing and its preparation method and application

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3296431A1 (en) * 2016-09-15 2018-03-21 Ecole Polytechnique Fédérale de Lausanne (EPFL) Method of synthesis of an electrode for use as a catalyst of oxygen evolution reaction
CN110518235A (en) * 2019-07-15 2019-11-29 广东工业大学 A kind of three nickel electrode of self-supporting curing and its preparation method and application

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
QING YAN ET AL.: "In Situ Formed Edge-Rich Ni3S2-NiOOH Heterojunctions for Oxygen Evolution Reaction", 《JOURNAL OF THEELECTROCHEMICAL SOCIETY》 *
闫卿: "镍基纳米材料的构筑及其电催化水分解性能研究", 《中国博士学位论文全文数据库 工程科技I辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114990619A (en) * 2022-05-25 2022-09-02 江苏大学 Amorphous NiOOH/Ni 3 S 2 Heterostructure type nickel-based composite catalyst and preparation method and application thereof
CN114990619B (en) * 2022-05-25 2023-12-15 江苏大学 Amorphous NiOOH/Ni 3 S 2 Nickel-based composite catalyst with heterojunction structure, preparation method and application thereof

Similar Documents

Publication Publication Date Title
CN109252180B (en) Ternary MOF nanosheet array material, preparation method and application thereof
CN111282582A (en) Preparation method of foam nickel-based catalyst for hydrogen production by water electrolysis
CN110639534B (en) Oxygen evolution electrocatalytic material and preparation method and application thereof
CN111001428B (en) Metal-free carbon-based electrocatalyst, preparation method and application
CN108435211B (en) Preparation method of Ce-doped Ni-Fe-Ce ternary sulfide oxygen evolution catalyst
CN111996543B (en) Vanadium-doped nickel selenide heterojunction self-supporting electrode and preparation method and application thereof
CN111939947B (en) Preparation method of nanosheet array electrocatalyst
CN112080759B (en) Preparation method of bismuth-doped bimetallic sulfide electrode for electrocatalytic oxidation of urea
CN115505961A (en) Low-cost catalytic electrode applied to rapid full-electrolysis hydrogen production of seawater, preparation and application
CN113667993A (en) Oxygen vacancy-rich cobalt monoxide/cobalt ferrite nanosheet array structure catalyst and preparation and application thereof
CN113846344A (en) Nickel disulfide oxygen evolution catalyst rich in edge active sites and preparation method thereof
CN116970974A (en) Preparation method of Ru/F-FeCoOOH heterojunction electrocatalyst based on hydrogen overflow strategy
CN109097788B (en) Double-carbon coupling transition metal nickel-based quantum dot electrocatalyst and preparation method thereof
CN108270017B (en) Nickel-nitrogen doped carbon composite material and preparation method and application thereof
CN114892206B (en) Multi-metal nitride heterojunction nanorod array composite electrocatalyst and preparation method and application thereof
CN116145176A (en) Method for preparing amorphous nickel-cobalt-iron sulfide nanosheet array oxygen evolution electrode in one step in situ
CN113981468B (en) Multi-dimensional nickel-cobalt-based sulfide heterojunction electrocatalytic composite material and preparation method thereof
CN109012683B (en) Preparation method of cobalt molybdate hollow microsphere electrocatalyst
CN115011997B (en) Self-supporting hollow sugarcoated haws-end electrocatalyst and preparation method and application thereof
CN115786964B (en) Cobalt-based spinel Cu 0.7 Co 2.3 O 4 Electrocatalyst, preparation method and application thereof
CN115125566B (en) Novel MOF-based oxygen evolution electrode material and preparation method and application thereof
CN114956019B (en) Method for one-step synthesis of cobalt phosphide by molten salt mediation and application thereof
CN117568862A (en) Catalyst for producing hydrogen by water electrolysis and preparation method and application thereof
CN116180128A (en) Self-supporting non-noble metal electrocatalyst material, and preparation method and application thereof
CN116676626A (en) Dual-function OER/HER water electrolysis catalyst, preparation method and application 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