CN112421065B - Carbon/molybdenum disulfide-sulfur molybdenum cobalt composite electrochemical catalyst material and preparation and application thereof - Google Patents
Carbon/molybdenum disulfide-sulfur molybdenum cobalt composite electrochemical catalyst material and preparation and application thereof Download PDFInfo
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- 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
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
Abstract
The invention discloses a carbon/molybdenum disulfide-sulfur molybdenum cobalt composite electrochemical catalyst material, and a preparation method and an application thereof, wherein the carbon/molybdenum disulfide-sulfur molybdenum cobalt composite electrochemical catalyst material is prepared from C/MoS2The nano-sheet and MOF material ZIF-67 are calcined and compounded at high temperature. The composite material has a large specific surface area and provides more catalytic active sites, so that the composite material has excellent catalytic performance when being used as a metal-air battery anode catalyst.
Description
Technical Field
The invention belongs to the field of metal-air batteries, and particularly relates to a C/MoS2-CoMo2S4A composite electrochemical catalyst material and preparation and application thereof.
Background
With the rapid development of life production and scientific technology, the consumption of energy is increasing day by day, the energy demand is increasingly short, and the problems of environmental pollution, resource shortage, greenhouse effect and the like caused by the large use of traditional fossil energy are increasingly prominent, so that the method becomes a major challenge for the development of human society. The conversion from fossil energy to clean renewable energy is not slow, and the development of novel, efficient and green new energy becomes a research and development hotspot in the energy field at home and abroad[1]. The metal-air battery has higher theoretical energy density and stable performance, and is a new chargeable technical fuel battery which can convert and store energy cleanly and efficiently.
The metal-air battery uses metal with more negative electrode potential, such as magnesium, aluminum, zinc, mercury, iron, etc. as the negative electrode, and oxygen or pure oxygen in the air as the active material of the positive electrode. The performance of metal-air batteries, such as charge and discharge efficiency, capacity retention rate, energy efficiency, cycle life, etc., depends on the Oxygen Reduction Reaction (ORR) during discharge and oxygen during charge of the oxygen electrode of the batteryPrecipitation reaction (OER) (O)2+4H2O+4e-→4OH-)[2]The two reactions involve multi-electron/proton transfer electrochemical reaction, and the process is slow and complex[3]. The performance of the metal-air battery can be improved by adding the catalyst material into the anode of the metal-air battery, for example, carbon-supported noble metal (such as Pt, Ru, Ir and the like) has good catalytic activity on ORR and OER, but the carbon-supported noble metal is expensive, cannot be used for industrial production and realizes large-scale commercialization[4]。
Transition metal sulfide materials have gained wide attention in the field of electrochemical energy storage and conversion due to their good electronic properties and relatively low economic cost. However, the limited number of active centers of the metal sulfide nanosheets, the easy aggregation due to strong van der waals forces, and the inherently slow charge transfer kinetics limit their application as positive electrode catalyst materials for metal-air batteries. Introduction of porous networks in materials to increase their surface area, in particular mesoporous metal polysulfides[5]The above problems can be solved. For example, P123 is used as a surfactant in seedlings and the like, the strategy of changing oxide to sulfide is expanded, and mesoporous pyrite FeS is synthesized2Nanoparticles[6]However, the resulting samples exhibit irregular morphology and the vapor phase oxide-sulfide conversion process is generally required to be at a high toxicity of H2And reacting for a long time under an S atmosphere. Therefore, it is very important to develop an efficient and cheap mesoporous metal polysulfide electrochemical catalyst.
Reference documents:
[1] tanyuqiang, hodeitin, Diandian and Liuyongning, a bifunctional catalyst for catalyzing ORR and OER, and preparation and application thereof [ P ]. Shanxi province: CN110148764A,2019-08-20.
[2] Von Jing, Chenjing, Xiaobing, development of metal air battery technology [ J ] materials report, 2005(10) 67-70.
[3] A high-efficiency dual-function oxygen electro-catalyst with a heterostructure, and preparation and application thereof [ P ]. Shanghai city: CN111729680A,2020-10-02.
[4] Bin, Zhang Min, Liupeng, et, bifunctional electrocatalyst for oxygen reduction and oxygen evolution reaction-nitrogen phosphorus-carbon-doped supported cobaltosic oxide [ J ] catalysis academic newspaper, 2016,37(8): 1249-.
[5]Guo Y,Tang J,Henzie J,et al.Mesoporous Iron-Doped MoS2/CoMo2S4Heterostructures through Organic-Metal Cooperative Interactions on Spherical Micelles for Electrochemical Water Splitting[J].ACS Nano,2020,14,4141-4152.
[6]Miao R,Dutta B,Sahoo S,He J,etal.Mesoporous iron sulfide for highly efficient electrocatalytic hydrogen evolution[J].J.Am.Chem.Soc.,2017,139,13604-13607.
Disclosure of Invention
Based on the problems of the prior art, the present invention aims to provide a C/MoS with simple preparation method and dual-function catalytic activity of ORR and OER2-CoMo2S4The composite electrochemical catalyst material and the preparation method thereof have good conductivity and catalytic activity, so that the electrochemical performance of the composite electrochemical catalyst material can be improved when the composite electrochemical catalyst material is used for a metal-air battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a carbon/molybdenum disulfide-sulfur molybdenum cobalt composite electrochemical catalyst material is characterized by comprising the following steps: the C/MoS2-CoMo2S4The composite electrochemical catalyst material is prepared from C/MoS2The nano-sheet and MOF material ZIF-67 are calcined and compounded at high temperature. The method comprises the following steps:
and 2, calcining the precursor precipitate in an inert atmosphere at 800-900 ℃ for 2-4 hours.
Further: in the solution A, C/MoS2The dosage ratio of the nanosheet to the organic solvent to the 2-methylimidazole is 0.3-0.7 g: 10mL of: 3-5 g; in the solution B, the dosage ratio of the metal cobalt salt, CTAB and the organic solvent is 1-2.5 g: 50-80 mg: 45 mL; the volume ratio of the solution A to the solution B is 1: 4.5.
further, the organic solvent is ethanol or methanol.
Further, the metal cobalt salt is cobalt chloride, cobalt bromide, cobalt carbonate, cobalt acetate or cobalt nitrate hexahydrate.
Further, the inert atmosphere is N2Or Ar2。
Further, the C/MoS2The nano-sheet is prepared by the following method: dissolving a molybdenum source, a carbon source and a sulfur source in distilled water, uniformly stirring, transferring to a reaction kettle, and reacting for 24-72 hours at 180-200 ℃; after the reaction is finished, the obtained product is filtered, washed to be neutral and dried to obtain the C-MoS2Nanosheets.
Further, the using amount ratio of the molybdenum source to the carbon source to the sulfur source to the distilled water is 1.5-2 g: 2-5 g: 0.8-4 g: 15-40 mL.
Further: the molybdenum source is ammonium molybdate tetrahydrate, molybdenum trioxide, calcium molybdate or molybdenum hexafluoride; the carbon source is glucose, sucrose or ethylene glycol; the sulfur source is thiourea, sulfur, mercaptan or methionine.
C/MoS prepared by the preparation method2-CoMo2S4The composite electrochemical catalyst material can be used as a metal-air battery anode catalyst material and has ORR and OER dual-function catalytic activity.
Compared with the prior art, the invention has the beneficial effects that:
1. the C/MoS provided by the invention2-CoMo2S4The composite material is composed ofZIF-67 and C/MoS2The nano-sheets are compounded under high-temperature calcination, and the metal Co nano-particles are exposed on the surface of the ZIF-67 material and are triggered at high temperature to form 1T/2H MoS2Nanoparticle modified amorphous Mo-CoSx frameworks. The composite material has a large specific surface area and provides more catalytic active sites, so that the composite material has excellent catalytic performance when being used as a metal-air battery anode catalyst.
2. C/MoS of the invention2-CoMo2S4In the composite material, ZIF-67 has the characteristics of porosity, controllable morphology and high specific surface area, and is doped with Co metal element and C-MoS2And a heterogeneous porous structure is formed under high-temperature carbonization, which is beneficial to the transportation of oxygen reaction products.
3. C/MoS of the invention2-CoMo2S4The composite material has good oxygen reduction (ORR) and Oxygen Evolution (OER) electrocatalytic activities in alkaline electrolyte, has potential application value in the fields of energy conversion and storage, and can be used for preparing a metal air battery with high energy density and good stability.
4. The preparation method has the advantages of simple process, easy operation and low cost.
Drawings
FIG. 1 is a C/MoS prepared in examples 1 to 42-CoMo2S4XRD contrast patterns of the composite materials, a to d represent the materials obtained in examples 1 to 4 in sequence;
FIG. 2 is a C/MoS prepared in example 12-CoMo2S4XPS plot of composite material;
FIG. 3 is an ORR performance test chart of the composite material prepared in example 1, wherein a to e sequentially represent test rotation speeds 2000, 1600, 1200, 800 and 400;
FIG. 4 is an ORR performance test chart of the composite materials prepared in examples 1 to 4, wherein a to d sequentially represent the materials obtained in examples 1 to 4;
FIG. 5 is an OER performance test chart of the composite materials prepared in examples 1-4, wherein a-d sequentially represent the materials obtained in examples 1-4.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
And 3, placing the precursor precipitate in a quartz boat, moving the quartz boat into a tube furnace, and calcining the quartz boat for 2 hours at 800 ℃ under the protection of argon.
Step 4, adding the product obtained in the step 3 into a 0.5mol/L sulfuric acid solution, condensing and refluxing for 3h at 90 ℃, carrying out suction filtration and washing on the obtained product to neutrality, and drying for 12h at 60 ℃ to obtain the target product C/MoS2-CoMo2S4A composite material.
Example 2
This example prepares a composite material in the same manner as in example 1 except that step 4 is not carried out.
Example 3
This example prepares a composite material in the same manner as in example 1 except that the calcination temperature in step 3 is 700 ℃.
Example 4
This example was carried out in the same manner as in example 2 to prepare C/MoS2-CoMo2S4The composite materials differ only in that the calcination temperature in step 3 is 700 ℃.
FIG. 1 is a C/MoS prepared in examples 1 to 42-CoMo2S4XRD contrast patterns of the composite materials, a to d represent the materials obtained in examples 1 to 4 in this order. The results show that: the product of example 1 successfully compounded CoMo compared to examples 2, 3, 42S4And C/MoS2And the characteristic peak is obvious; product CoMo of example 22S4The strength of the characteristic peak is weaker, which indicates that the acid washing can wash off some impurities in the product, so that the characteristic peak is obvious; the products of examples 3, 4 do not have significant CoMo2S4And C/MoS2Indicating that calcination at 700 ℃ did not form CoMo2S4。
FIG. 2 is a C/MoS prepared in example 12-CoMo2S4XPS (X-ray diffraction) diagram of composite material, and the diagram shows that the obtained material is successfully compounded with CoMo2S4And C/MoS2。
The ORR and OER properties of the composites prepared in the above examples were tested as follows: 2mg of the catalyst, 0.4mg of Ketjen black KB and 15. mu.L of naphthol were dissolved together in 1000. mu.L of an aqueous ethanol solution (ethanol: water: 1:4) and sonicated for 1h to obtain a homogeneous mixed solution. And dripping 10 mu L of mixed solution on a glassy carbon electrode, air-drying for 2h to form a catalyst layer, and carrying out an LSV test on a disc electrode.
FIG. 3 is a graph showing ORR performance test of the composite material prepared in example 1 at different rotation speeds. FIGS. 4 and 5 are ORR performance comparison plots (1600 rpm) and OER performance comparison plots (1600 rpm) for the composite materials prepared in examples 1 to 4, respectively, and a to d sequentially represent the materials obtained in examples 1 to 4. The results show that: compared with examples 2, 3 and 4, the product of example 1 has higher limiting current density and lower overpotential, has good ORR and OER performances, can be applied to a metal air battery, and improves the energy density and the cycling stability of the battery by catalyzing the oxygen reaction.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A preparation method of a carbon/molybdenum disulfide-sulfur molybdenum cobalt composite electrochemical catalyst material is characterized by comprising the following steps: the carbon/molybdenum disulfide-sulfur molybdenum cobalt composite electrochemical catalyst material is prepared from C/MoS2The nano-sheet and MOF material ZIF-67 are calcined and compounded at high temperature, and the method specifically comprises the following steps:
step 1, mixing C/MoS2Adding the nanosheets into an organic solvent, uniformly dispersing by ultrasonic, adding 2-methylimidazole, and uniformly dispersing by ultrasonic to obtain a solution A; dissolving metal cobalt salt and CTAB in an organic solvent to obtain a solution B; dropwise adding the solution A into the solution B, uniformly stirring, carrying out water bath reaction at 50-60 ℃ for 1h, standing for 12-24 h, centrifuging, and drying to obtain a precursor precipitate;
step 2, calcining the precursor precipitate in an inert atmosphere at 800-900 ℃ for 2-4 hours;
and 3, adding the product obtained in the step 2 into a 0.5mol/L sulfuric acid solution, condensing and refluxing for 3 hours at 70-90 ℃, carrying out suction filtration, washing to be neutral, and drying on the obtained product to obtain the target product, namely the carbon/molybdenum disulfide-sulfur molybdenum cobalt composite electrochemical catalyst material, which is marked as C/MoS2-CoMo2S4A composite electrochemical catalyst material.
2. The method of claim 1, wherein: in the solution A, C/MoS2The dosage ratio of the nanosheet to the organic solvent to the 2-methylimidazole is 0.3-0.7 g: 10mL of: 3-5 g;
in the solution B, the dosage ratio of the metal cobalt salt, CTAB and the organic solvent is 1-2.5 g: 50-80 mg: 45 mL;
the volume ratio of the solution A to the solution B is 1: 4.5.
3. the method of claim 1, wherein: the organic solvent is ethanol or methanol.
4. The method of claim 1, wherein: the metal cobalt salt is cobalt chloride, cobalt bromide, cobalt carbonate, cobalt acetate or cobalt nitrate hexahydrate.
5. The method of claim 1, wherein: the inert atmosphere is N2Or Ar2。
6. The method of claim 1, wherein: the C/MoS2The nano-sheet is prepared by the following method: dissolving a molybdenum source, a carbon source and a sulfur source in distilled water, uniformly stirring, transferring to a reaction kettle, and reacting for 24-48 h at 180-200 ℃; after the reaction is finished, the obtained product is filtered, washed to be neutral and dried to obtain the C-MoS2Nanosheets.
7. The method of claim 6, wherein: the using amount ratio of the molybdenum source to the carbon source to the sulfur source to the distilled water is 1.5-2 g: 2-5 g: 0.8-4 g: 15-40 mL.
8. C/MoS prepared by the preparation method of any one of claims 1 to 72-CoMo2S4A composite electrochemical catalyst material.
9. C/MoS according to claim 82-CoMo2S4The composite electrochemical catalyst material is applied as a metal-air battery anode catalyst material.
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