CN113549930B - Preparation method of high-activity OER and ORR catalyst - Google Patents
Preparation method of high-activity OER and ORR catalyst Download PDFInfo
- Publication number
- CN113549930B CN113549930B CN202110862542.XA CN202110862542A CN113549930B CN 113549930 B CN113549930 B CN 113549930B CN 202110862542 A CN202110862542 A CN 202110862542A CN 113549930 B CN113549930 B CN 113549930B
- Authority
- CN
- China
- Prior art keywords
- solution
- mxene
- deionized water
- preparation
- stirring
- 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
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—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
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
-
- 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
-
- 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
-
- 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
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
-
- 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
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
-
- 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)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of high-activity catalytic materials, and particularly relates to a preparation method of high-activity OER and ORR catalysts. The preparation method is to mix Ni (OH) by a simple wet chemical method 2 The nanosheet directly and vertically grows on MXene to prepare the catalyst with high activity OER and ORR. The preparation method is simple to operate and easy to control; the raw materials in the preparation process are cheap and basically harmless chemicals such as metal nitrate, the cost can be reduced, and the industrial production is facilitated.
Description
Technical Field
The invention belongs to the technical field of high-activity catalytic materials, and particularly relates to a preparation method of high-activity OER and ORR catalysts.
Background
With the increasing emphasis on energy crisis and environmental issues, energy storage and conversion technologies, such as metal-air batteries, photo-electrolysis water and fuel cells, have received increasing attention. Electrocatalytic oxygen evolution and oxygen reduction are very important reaction processes in energy conversion technology, but the reaction electrochemical process of air electrode discharge reaction ORR (oxygen reduction reaction) and air electrode charging reaction OER (oxygen evolution reaction) is quite complex, a series of slow-kinetic multi-step electron transfer electrochemical reactions are involved, and the reaction potential window is wide, so that the reactions generally have large overpotentials and poor reversibility. Meanwhile, a considerable amount of peroxide byproducts are generated in the ORR reaction process, so that the catalytic efficiency is reduced, the service life of a battery diaphragm is influenced, and finally the energy density and the service life of the metal-air battery are influenced.
The electrocatalyst can effectively reduce electrochemical polarization and has a vital effect on accelerating oxygen electrochemical reaction and improving battery capacity. The traditional Pt, ru and Ir-based catalysts have good catalytic activity for ORR and OER, but are limited by high price and extremely limited reserves, and are difficult to realize commercialization on a large scale. Therefore, there is a need to find and develop a non-noble metal catalyst with high activity, high selectivity and high stability.
Disclosure of Invention
The invention aims to provide a preparation method of high-activity OER and ORR catalysts, aiming at the defects, and the preparation method is simple to operate and easy to control; the raw materials in the preparation process are cheap and basically harmless chemicals such as metal nitrate, the cost can be reduced, and the industrial production is facilitated.
The technical scheme of the invention is as follows: a preparation method of high-activity OER and ORR catalysts comprises the steps of firstly dispersing MXene in deionized water for ultrasonic treatment to obtain MXene solution; then adding Ni (NO) 3 ) 2 ·6H 2 Dissolving O in MXene solution, stirring to obtain mixed solution, adding C 6 H 5 O 7 Na 3 Adding deionized water solution of HMTA and the mixed solution into the mixed solution, stirring, heating the solution to 80-90 ℃, keeping the solution for 8-10 hours under the stirring condition, cooling the solution to room temperature, centrifuging, washing and drying to obtain Ni (OH) 2 Nano array vertical growth Ni (OH) on two-dimensional MXene 2 -MXene composite material.
The MXene is 10-50 mg and is dispersed in 50mL of deionized water; ni (NO) 3 ) 2 ·6H 2 O is 2.5mmol; containing C 6 H 5 O 7 Na 3 And HMTA in 50mL deionized water containing C 6 H 5 O 7 Na 3 0.25mmol and 2.5mmol HMTA.
The ultrasonic treatment time is 1-2 hours; ni (NO) 3 ) 2 ·6H 2 The dissolving and stirring time of O is 0.5 to 1 hour; adding the deionized water solution into the mixed solution, and stirring for 1-2 hours; the solution was heated and stirred at 500rmp.
The washing adopts deionization; the drying was freeze-dried at-50 ℃ for 24 hours.
The MXene is d-MXene.
The MXene is Ti 3 C 2 T x 、Ti 2 CT x 、Cr 2 CT x 。
The beneficial effects of the invention are as follows: the preparation method of the high-activity OER and ORR catalyst adopts the reasonable design of a transition metal nickel hydroxide nano array on MXene to obtain the catalyst. By simple wet-chemical method Ni (OH) 2 The nanosheet directly and vertically grows on MXene to prepare the catalyst with high activity OER and ORR.
In the catalyst composite material prepared by the preparation method, MXene nano-flake is Ni (OH) 2 Provide steric hindrance to the nucleation and growth of (A) so that Ni (OH) 2 The active carbon directly and vertically grows on the hydroxyl-rich surface of MXene, effectively prevents self aggregation, exposes more edge active centers and shows higher specific surface area. More importantly, ni (OH) 2 And MXene, and the composite material becomes an excellent ORR/OER electrocatalyst under the synergistic action of the two materials.
(2) The preparation method obtains the catalyst through constant-temperature solvothermal reaction, centrifugal washing and freeze drying, and is simple to operate and easy to control; the raw materials in the preparation process are cheap and basically harmless chemicals such as metal nitrate, the cost can be reduced, and the industrial production is facilitated.
Drawings
FIG. 1 shows Ni (OH) obtained in example 1 2 SEM image of MXene composite material.
FIG. 2 shows Ni (OH) obtained in example 1 2 -MXene composite material used in electrocatalytic OER and ORR graphs.
Detailed Description
The technical scheme of the invention is explained in detail in the following with reference to the attached drawings.
Example 1
The preparation method of the high-activity OER and ORR catalyst comprises the steps of firstly dispersing 23.18mg of d-MXene in 50mL of deionized water, and carrying out ultrasonic treatment for 1 hour to obtain MXene solution; then 2.5mmolNi (NO) is added 3 ) 2 ·6H 2 Dissolving O in MXene solution, stirring for 1 hr to obtain mixed solution, adding water to obtain solution containing 0.25mmol C 6 H 5 O 7 Na 3 Adding 50mL of deionized water solution of 2.5mmol HMTA into the mixed solution, stirring for 2 hours, heating the obtained solution to 90 ℃, keeping the solution for 9 hours under the stirring condition of the rotation speed of 500rmp, cooling the solution to room temperature, and centrifuging to collect a product; washing with deionized water; freeze drying at-50 deg.C for 24h to obtain Ni (OH) 2 Nano array vertical growth Ni (OH) on two-dimensional MXene 2 -MXene (nickel hydroxide nanosheet array-MXene) composite.
As can be seen from FIG. 1, ni (OH) 2 The nanoarrays are grown vertically on two-dimensional MXene.
Example 2
The preparation method of the high-activity OER and ORR catalyst comprises the steps of firstly dispersing 12mg of d-MXene in 50mL of deionized water, and carrying out ultrasonic treatment for 2 hours to obtain an MXene solution; then 2.5mmolNi (NO) is added 3 ) 2 ·6H 2 Dissolving O in MXene solution, stirring for 1 hr to obtain mixed solution, adding water to obtain solution containing 0.25mmol C 6 H 5 O 7 Na 3 And 2.5 mmole HMTA in 50mL of deionized water was added to the above mixed solution and stirred for 1 hour, and the resulting solution was heated to 85 ℃ with a stirring bar at 500rmpKeeping for 10 hours, cooling the solution to room temperature, and centrifuging to collect a product; washing with deionized water; freeze drying at-50 deg.C for 24h to obtain Ni (OH) 2 -MXene (nickel hydroxide nanosheet array-MXene) composite.
Example 3
The preparation method of the high-activity OER and ORR catalyst comprises the steps of firstly dispersing 46.36mg of d-MXene in 50mL of deionized water, and carrying out ultrasonic treatment for 1 hour to obtain MXene solution; then 2.5mmolNi (NO) is added 3 ) 2 ·6H 2 Dissolving O in MXene solution, stirring for 1 hr to obtain mixed solution, adding water to obtain solution containing 0.25mmol C 6 H 5 O 7 Na 3 Adding 50mL of deionized water solution of 2.5mmol HMTA into the mixed solution, stirring for 2 hours, heating the obtained solution to 80 ℃, keeping the solution for 10 hours under the stirring condition of the rotation speed of 500rmp, cooling the solution to room temperature, and centrifuging to collect a product; washing with deionized water; freeze drying at-50 deg.C for 24h to obtain Ni (OH) 2 -MXene (nickel hydroxide nanosheet array-MXene) composite.
Claims (1)
1. A preparation method of high-activity OER and ORR catalysts is characterized in that,
firstly, dispersing MXene in deionized water and carrying out ultrasonic treatment to obtain MXene solution;
then adding Ni (NO) 3 ) 2 ·6H 2 Dissolving O in MXene solution, stirring to obtain mixed solution, adding C 6 H 5 O 7 Na 3 Adding deionized water solution of HMTA and the mixed solution into the mixed solution, stirring, heating the solution to 80-90 ℃, keeping the solution for 8-10 hours under the stirring condition, cooling the solution to room temperature, centrifuging, washing and drying to obtain Ni (OH) 2 Nano array vertical growth Ni (OH) on two-dimensional MXene 2 -MXene composite;
the MXene is 10-50 mg and is dispersed in 50mL of deionized water; ni (NO) 3 ) 2 ·6H 2 O is 2.5mmol; containing C 6 H 5 O 7 Na 3 And HMTA in 50mL deionized water containing C 6 H 5 O 7 Na 3 0.25mmol, HMTA 2.5mmol;
the ultrasonic treatment time is 1-2 hours; ni (NO) 3 ) 2 ·6H 2 The dissolving and stirring time of O is 0.5 to 1 hour; adding the deionized water solution into the mixed solution, and stirring for 1-2 hours; the heating and stirring speed of the solution is 500 rmp;
deionized water is adopted for washing; drying by freeze drying at-50 deg.C for 24 hr;
the MXene is Ti 3 C 2 T x 、Ti 2 CT x 、Cr 2 CT x 。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110862542.XA CN113549930B (en) | 2021-07-29 | 2021-07-29 | Preparation method of high-activity OER and ORR catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110862542.XA CN113549930B (en) | 2021-07-29 | 2021-07-29 | Preparation method of high-activity OER and ORR catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113549930A CN113549930A (en) | 2021-10-26 |
| CN113549930B true CN113549930B (en) | 2023-03-07 |
Family
ID=78133226
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110862542.XA Active CN113549930B (en) | 2021-07-29 | 2021-07-29 | Preparation method of high-activity OER and ORR catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113549930B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114649536B (en) * | 2022-03-21 | 2023-06-23 | 河北工业大学 | Rare earth oxide loaded iron nanoparticle catalyst and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112467068A (en) * | 2020-12-11 | 2021-03-09 | 燕山大学 | Battery negative electrode material and preparation method and application thereof |
-
2021
- 2021-07-29 CN CN202110862542.XA patent/CN113549930B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112467068A (en) * | 2020-12-11 | 2021-03-09 | 燕山大学 | Battery negative electrode material and preparation method and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| 0D/2D NiS2/V-MXene composite for electrocatalytic H2 evolution;Panyong Kuang et al;《Journal of Catalysis》;20190731;第8-20页 * |
| Atomic Insights of Iron Doping in Nickel Hydroxide Nanosheets for Enhanced Oxygen Catalysis to Boost Broad Temperature Workable Zinc- Air Batteries;Rui Yang et al;《ChemPubSoc》;20191006;第1-7页 * |
| Recent advances in MXene-based nanoarchitectures as electrode materials for future energy generation and conversion applications;Cuizhen Yang et al;《Coordination Chemistry Reviews》;20210212;第1-32页 * |
| Synthesis of nickel hydroxide/delaminated-Ti3C2 MXene nanosheets as promising anode material for high performance lithium ion battery;Chenyang Li et al;《Journal of Alloys and Compounds》;20200530;第1-7页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113549930A (en) | 2021-10-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110380062B (en) | Preparation method of sulfur-doped bifunctional oxygen catalyst based on ZIF-67 and conductive graphene | |
| CN110479329B (en) | Preparation and application of phosphorus-doped cobalt telluride nano material | |
| CN108325539A (en) | A kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2The synthetic method of elctro-catalyst | |
| CN111013615A (en) | Preparation method of CoP catalyst with hydrogen precipitation and oxygen precipitation high-efficiency dual functions | |
| CN115896807B (en) | Electrocatalytic water oxidation homogeneous diatomic catalyst, and preparation method and application thereof | |
| CN113549930B (en) | Preparation method of high-activity OER and ORR catalyst | |
| CN109647536B (en) | Cobalt-nickel double-doped tin sulfide nanosheet as well as preparation method and application thereof | |
| CN112838224B (en) | Proton exchange membrane fuel cell membrane electrode anti-reversal additive and preparation method thereof | |
| CN112076764A (en) | Preparation method and application of nickel-doped pyrrhotite FeS nanoparticles | |
| CN111933955A (en) | Preparation method of surface carbon-supported platinum-cobalt alloy electrocatalyst with high electrochemical activity | |
| CN116288474A (en) | CuO@Cu for electrocatalytic reduction of carbon dioxide to ethylene 2 Preparation method of O composite catalyst | |
| CN109097788B (en) | Double-carbon coupling transition metal nickel-based quantum dot electrocatalyst and preparation method thereof | |
| CN108842165B (en) | Solvothermal preparation of sulfur doped NiFe (CN)5NO electrolysis water oxygen evolution catalyst and application thereof | |
| CN113122876B (en) | Preparation method and application of molybdenum-doped ferronickel Prussian blue analogue @ carbon felt | |
| CN116180107A (en) | Amorphous nickel iron tungstate catalytic material and preparation method and application thereof | |
| CN114709436B (en) | Has Fe2Preparation and application of oxygen evolution/hydrogen evolution/oxygen reduction electrocatalyst with P/Co nano particle synergistic effect | |
| CN115896809A (en) | Supported IrRu alloy nanosheet catalyst and preparation method thereof | |
| CN114108005A (en) | Preparation method of nickel cobalt hydroxide nanosheet and prepared nickel cobalt hydroxide nanosheet | |
| CN110882698B (en) | Preparation and application of novel electrocatalyst | |
| CN113437312A (en) | Preparation of Prussian blue derivative catalyst applied to zinc-air battery | |
| CN114232017B (en) | Silver selenide nano catalyst and preparation method and application thereof | |
| CN114291798B (en) | Cobalt telluride nano rod electrocatalyst synthesized by microwave method and application thereof | |
| KR102362247B1 (en) | Preparation method of catalyst for PEM hydrolysis and catalyst for PEM hydrolysis | |
| CN117512670A (en) | Electro-catalyst for preparing hydrogen from methanol and preparation method thereof | |
| CN115976542A (en) | Single noble metal doping construction dual-active-site catalyst and 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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |