CN111063895A - Non-carbon-based air electrode material for rechargeable zinc-air battery - Google Patents
Non-carbon-based air electrode material for rechargeable zinc-air battery Download PDFInfo
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- CN111063895A CN111063895A CN201811213401.XA CN201811213401A CN111063895A CN 111063895 A CN111063895 A CN 111063895A CN 201811213401 A CN201811213401 A CN 201811213401A CN 111063895 A CN111063895 A CN 111063895A
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- 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
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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
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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
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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Abstract
The invention relates to an air electrode material of a zinc-air battery, in particular to a non-carbon-based air electrode material which uses a carbide-supported high-efficiency catalyst as a rechargeable zinc-air battery, an air electrode containing the material is prepared, and the air electrode material is applied to the rechargeable zinc-air battery. The preparation method is simple to operate, the prepared non-carbon-based air electrode material takes the carbide as a carrier, and the carbide has good conductivity, particularly high chemical (no reaction with acidic and alkaline solutions) and electrochemical stability in the operation process, so that the high cycle stability of the zinc-air battery is realized, and high power density can be realized by further loading a high-efficiency catalyst.
Description
(I) technical field
The invention relates to an air electrode material of a zinc-air battery, in particular to a non-carbon-based air electrode using carbide (boron carbide, titanium carbide, tungsten carbide and the like) as a rechargeable zinc-air batteryAnd the electrode material realizes high cycle stability of the zinc-air battery. By further loading a high efficiency catalyst (e.g., MnO)2，Co3O4Etc.) can achieve high power densities.
(II) background of the invention
With the rising of fossil energy and the increasingly prominent environmental problems, more and more countries in the world are actively pushing the development of electric vehicles to reduce the dependence of economic and social development on fossil fuels and establish a sustainable energy system based on renewable energy. As a promising technology, the lithium ion battery is widely applied to commercial electric vehicles at present, but the energy density of the lithium ion battery is 100-150 Wh kg-1) Still far below the requirements of electric vehicles. In the next generation of energy storage conversion devices, zinc air cells (ZAB) are used for their excellent economy and potentially high energy density (1086Wh kg)-1) But is of great interest. The development of rechargeable zinc-air cells with long cycle life and high energy efficiency depends to a large extent on the performance of the electrocatalyst in the air cathode. Since the commercial ZAB was first introduced in the 30's last century, the air electrode catalyst has rapidly developed in the kinetics of Oxygen Reduction Reaction (ORR) and Oxygen Evolution Reaction (OER), but due to the use of noble metals (such as Pt, Ir, Ru, etc.) and electrochemically unstable carbon materials, the ZAB has a short charge-discharge life and low energy efficiency, which has severely hindered the commercialization of ZAB.
Carbon-based materials have been widely used as air electrode materials for zinc-air batteries so far due to their high electrical conductivity and abundant active centers. However, the carbon-based material is unstable under the operating conditions of the ZAB, and is easily corroded by repeated discharge and charge oxidation in a high-concentration alkaline electrolyte, so that the carbon material in the air cathode is oxidized into carbonate to react with the electrolyte, or the carbon material is continuously oxidized to generate carboxylic acid, so that the conductivity of the electrolyte is reduced, the air electrode fails, and the ZAB cannot perform charge-discharge cycles.
The present invention is directed to the development of high power density, high energy density and long life ZAB using carbides with low cost, ultra-high chemical and electrochemical stability, and high ORR and OER activityThe base material (such as boron carbide, titanium carbide, tungsten carbide and the like) is used as the non-carbon-based air electrode material of the ZAB, so that the problems of chemical corrosion of the carbon material in strong alkaline electrolyte and electrochemical corrosion in the charging process of the ZAB are solved, and the long-time and high-efficiency charge-discharge cycle of the ZAB under high energy density is realized. The invention further uses carbide as a carrier to load ORR and OER electro-catalysts with low cost and high activity, thereby further improving the cycle efficiency of ZAB. The carbide has good conductivity, and ultrahigh chemical (no reaction with acidic and alkaline solutions) and electrochemical stability under ZAB working conditions, is a very efficient and practical zinc-air battery electrode material, can realize high cycle stability of ZAB, and can be further loaded with a low-cost high-efficiency catalyst (such as MnO)2，Co3O4Etc.) can further achieve high power and energy densities of ZAB.
Disclosure of the invention
The invention aims to provide a non-carbon-based air electrode material with high activity and high stability for a rechargeable zinc-air battery, in particular to a method for preparing a non-carbon-based air electrode material by using carbide (such as boron carbide, titanium carbide, tungsten carbide and the like) and a carbide-supported low-cost high-efficiency catalyst (such as MnO)2，Co3O4Etc.) as a non-carbon-based air electrode material of a rechargeable zinc-air battery, high cycle stability and high power and energy density of the zinc-air battery are achieved.
The invention provides a high-activity and high-stability non-carbon-based air electrode material, in particular to a carbide material such as boron carbide, titanium carbide, tungsten carbide and the like which has high chemical and electrochemical stability and high ORR and OER activity.
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) is loaded in a carbide (boron carbide, titanium carbide, tungsten carbide, etc.) as a non-carbon-based air electrode material of a rechargeable zinc-air battery, firstly, a proper amount of cobalt salt or manganese salt and an organic ligand (such as: urea, citric acid, ethylene glycol, etc.) until a clear solution is obtained. Then adding proper amount of carbonAnd (3) stirring the compound (boron carbide, titanium carbide, tungsten carbide and the like) at room temperature for 2-8 hours at the stirring temperature of 30-80 ℃ and the rotating speed of 100-1000 rpm, transferring the precursor solution into a hydrothermal reaction kettle, and putting the hydrothermal reaction kettle into an oven for hydrothermal synthesis reaction.
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) is loaded on carbide (boron carbide, titanium carbide, tungsten carbide, etc.) to be used as a non-carbon-based air electrode material of a rechargeable zinc-air battery, catalyst powder is prepared by a hydrothermal synthesis method, the heating temperature is 60-140 ℃, and the heating time is 2-12 hours.
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) is loaded in a carbide (boron carbide, titanium carbide, tungsten carbide, etc.) to be used as a non-carbon-based air electrode material of a rechargeable zinc-air battery, catalyst powder is prepared by a hydrothermal synthesis method, the obtained material is collected by a centrifugal method after being cooled, washed three times by water and alcohol, and dried by a vacuum oven at room temperature.
The invention provides a catalyst based on carbide (such as boron carbide, titanium carbide, tungsten carbide and the like) and high-efficiency catalyst (such as MnO)2，Co3O4Etc.) the non-carbon-based air electrode of the rechargeable zinc-air battery prepared by loading carbide comprises the following specific preparation methods: the air electrode is composed of carbide-based catalyst powder, a binder and the like. Firstly, catalyst powder and pore-forming agent are mixed with binder in organic solvent (such as ethanol, acetone, isopropanol and the like) or mixed solvent of the organic solvent and deionized water, and uniform slurry is formed by ultrasonic and violent stirring. The mass ratio of the catalyst to the binder is 60: 40-97: 3. The slurry is vigorously stirred and then applied to a current collector by spraying, coating, printing, etc. to form an electrode. Drying the electrode in a vacuum oven at 30-100 deg.C for 3-24 hr, and placing in a tube furnace in inert atmosphere (such as Ar, He, N)2And the like), annealing at 100-350 ℃ for 0.5-3 hours, and removing the pore-forming agent to obtain the air electrode.
The invention provides a high-efficiency catalyst (such as M)nO2，Co3O4Etc.) in a carbide (e.g.: boron carbide, titanium carbide, tungsten carbide, etc.) as a non-carbon-based air electrode material of a rechargeable zinc-air battery, the binder used in preparing the positive electrode slurry is organic or aqueous binder such as PTFE, PVDF, CMC, starch, etc.
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) in a carbide (e.g.: boron carbide, titanium carbide, tungsten carbide, etc.) as the non-carbon-based air electrode material of the rechargeable zinc-air battery, activated carbon, graphite, starch, NH and the like are adopted in the preparation method of the positive electrode slurry4HCO3And the powder is used as a pore forming agent, and the content of the powder is 5-50% of the total mass of the catalyst powder and the PTFE.
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) in a carbide (e.g.: boron carbide, titanium carbide, tungsten carbide and the like) as a non-carbon-based air electrode material of the rechargeable zinc-air battery, and the substrate of the non-carbon-based air electrode current collector adopted in the preparation of the positive electrode material can be a titanium mesh, a nickel mesh, a stainless steel mesh, foamed nickel and the like.
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) in a carbide (e.g.: boron carbide, titanium carbide, tungsten carbide, etc.) as a non-carbon-based air electrode for a rechargeable zinc-air battery, with particular application in assembling rechargeable zinc-air batteries. The electrolyte comprises an air battery mould, a positive electrode material, electrolyte, a zinc negative electrode material, a sealing element, a fastening element and the like.
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) in a carbide (e.g.: boron carbide, titanium carbide, tungsten carbide, etc.) as a non-carbon-based air electrode material of a rechargeable zinc-air battery, the thickness of the zinc sheet used in assembling the battery may be 0.1 to 1 mm.
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) in a carbide (e.g.: boron carbide and carbonTitanium carbide, tungsten carbide and the like) as a non-carbon-based air electrode material of a rechargeable zinc-air battery, the typical loading amount of the catalyst and the PTFE combined air electrode is 1-10 mg cm-2. The geometric area of the air electrode is about 0.3-5 cm2。
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) in a carbide (e.g.: boron carbide, titanium carbide, tungsten carbide, etc.) as a non-carbon-based air electrode material of a rechargeable zinc-air battery, 1-6M KOH and 0.1-0.5M Zn (CH) are used as electrolytes3COO)2。
The invention provides a high-efficiency catalyst (such as MnO)2，Co3O4Etc.) in a carbide (e.g.: boron carbide, titanium carbide, tungsten carbide and the like) as a non-carbon-based air electrode material of a rechargeable zinc-air battery, and the application thereof.
(IV) description of the drawings
FIG. 1 α -MnO2ORR performance diagram of/TiC cathode material
FIG. 2 discharge polarization curve and power density diagram of zinc-air battery
FIG. 3 is a graph of the charge-discharge cycle performance of a zinc-air battery
FIG. 4 energy density diagram of zinc-air cell
(V) detailed description of the preferred embodiments
The following examples further illustrate the invention but are not intended to limit the invention thereto.
Example 1
When preparing the catalyst powder, 0.003M MnSO is firstly added into 20mL of glycol solution4H2O (or 0.09MCo (OAC)2·4H2O) and 0.18M urea, magnetically stirring until a clarified product is obtainedAdding a proper amount of carbide (such as boron carbide, titanium carbide, tungsten carbide and the like) into the clear solution, stirring until the mixture is uniformly mixed, stirring the mixture at room temperature for 0-12 hours at the stirring temperature of 30-80 ℃ and the rotating speed of 200-800 rpm, transferring the precursor solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, carrying out hydrothermal synthesis reaction at the heating temperature of 50-140 ℃, and heating for 3-12 hours. After cooling, the obtained material was collected by centrifugation, washed three times with water and three times with alcohol, and dried in a vacuum oven at room temperature to obtain powder.
Example 2
In evaluating the ORR performance of the catalyst, the electrochemical performance of the cell was tested at room temperature in a 0.1M KOH-filled standard three-electrode electrochemical cell. To prepare the working electrode, the catalyst, distilled water, ethanol and 5% Nafion solution were mixed in the appropriate ratio and the resulting mixture was sonicated to form a uniform suspension. The catalyst ink (5. mu.L) was then placed on a glassy carbon electrode (5 mm diameter, 0.196 cm)2) And drying at room temperature. Taking a Pt sheet and a saturated calomel electrode (saturated KCl) as a counter electrode and a reference electrode respectively, and the scanning rate is 5mVs-1Electrochemical tests were performed on the CHI760E electrochemical workstation. Before each experiment, pure oxygen (99.9%) is introduced into the electrolyte for 30-60 min to saturate the electrolyte with oxygen in the experiment process. The specific experimental results are shown in FIG. 1.
Example 3
Experiment in preparing air electrode slurry, the ratio of catalyst to binder was 9: 1. Firstly, weighing a certain amount of carbide-based catalyst powder and NH4HCO3Adding isopropanol and deionized water (the mass ratio is 2: 1) to perform ultrasonic mixing uniformly, and then dropwise adding Polytetrafluoroethylene (PTFE) to mix to form slurry. The sonication was continued until a homogeneous slurry was formed, which was then coated on a 316 stainless steel wire mesh (100 mesh) to form an electrode. Drying the electrode in a vacuum oven at 30-80 ℃ for 3-24 hours, and introducing N into a tube furnace2And annealing at 100-350 ℃ for 0.5-3 hours, and removing the pore-forming agent to obtain the air electrode of the rechargeable zinc-air battery.
Example 4
Test on the implementation of chargeable zincWhen the battery is assembled, the anode material is titanium mesh, nickel mesh, stainless steel mesh, foam nickel and the like coated with the air electrode material. The electrolyte is 1-8M KOH and 0.1-0.5M Zn (CH)3COO)2. The cathode material is a zinc sheet, and the thickness of the zinc sheet is 0.1-1 mm.
Example 5
Tests the assembled cells were subjected to performance tests. When the battery is tested, firstly, the open-circuit voltage of the battery is tested, and then the battery is subjected to a discharge polarization curve and power density test, wherein specific experimental results are shown in fig. 2. Then, the battery is subjected to charge-discharge cycle performance test, and the current density is 10mAcm-2And the charge and discharge time was 10 minutes, respectively, and a cycle performance test was performed, as shown in fig. 3. The cells were subjected to energy density performance tests, see fig. 4.
Claims (5)
1. A non-carbon based air electrode material for a rechargeable zinc-air battery, characterized by: using highly conductive, chemically and electrochemically stable carbide (boron carbide, titanium carbide, tungsten carbide, etc.) materials and carbide-supported low-cost high-efficiency catalysts (e.g., MnO)2，Co3O4Etc.) materials prepared into air electrodes comprising the same, for application to rechargeable zinc-air batteries.
2. The carbide (such as boron carbide, titanium carbide, tungsten carbide, etc.) and the carbide supported low-cost high-efficiency catalyst (such as MnO) for rechargeable zinc-air battery according to claim 12，Co3O4Etc.) non-carbon-based air electrode material and a preparation method of an air electrode containing the material, which is characterized in that: the air electrode material powder is prepared by using carbide as an air electrode material or loading a low-cost high-efficiency catalyst through the carbide. In the preparation process of the carbide supported catalyst material, metal salt compounds such as manganese salt and cobalt salt, organic ligands such as urea, citric acid and ethylene glycol and carbide are used as raw materials, a hydrothermal synthesis reaction method is utilized, and ethylene glycol is used as a solvent. Firstly, adding a proper amount of metal salt compound and organic ligand into a proper amount of organic or aqueous solutionAnd magnetically stirring until a clear solution is obtained, adding a proper amount of carbide (such as boron carbide, titanium carbide, tungsten carbide and the like), stirring the mixture at room temperature for 0.5-12 hours at the stirring temperature of 30-80 ℃ and the rotating speed of 100-800 rpm, transferring the precursor solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, carrying out hydrothermal synthesis reaction, cooling, washing, filtering, centrifuging and drying to obtain powder.
3. The carbide (such as boron carbide, titanium carbide, tungsten carbide, etc.) and the carbide supported low-cost high-efficiency catalyst (such as MnO) for rechargeable zinc-air battery according to claim 12，Co3O4Etc.) non-carbon-based air electrode material and a preparation method of an air electrode containing the material, which is characterized in that:
(1) when the air electrode slurry is prepared, the catalyst powder and the pore-forming agent are mixed with an organic or aqueous binder (such as Polytetrafluoroethylene (PTFE), PVDF, CMC, starch and the like) in an organic solvent (such as ethanol, isopropanol, acetone and the like) and deionized water or a mixed solvent thereof to form the slurry, wherein the mass ratio of the catalyst to the PTFE is 60: 40-97: 3.
(2) The slurry is vigorously stirred, sonicated until a uniform slurry is formed, and then coated on a current collector to form an electrode. Drying the electrode in a vacuum oven at 30-100 deg.C for 3-24 hr, introducing inert gas (such as Ar, He, N) into the tube furnace2And the like) annealing at 100-300 ℃ for 0.5-3 hours, and removing the pore-forming agent to obtain the air electrode.
4. A carbide (e.g. boron carbide, titanium carbide, tungsten carbide, etc.) and a carbide-supported low-cost high-efficiency catalyst (e.g. MnO) for rechargeable zinc-air battery according to claim 32，Co3O4Etc.) non-carbon-based air electrode material and a preparation method of an air electrode containing the material, which is characterized in that: in the step (1), activated carbon, graphite, starch and NH are used4HCO3And the powder is used as a pore forming agent, and the content of the powder is 5-40% of the total mass of the catalyst and the PTFE.
5. The carbide (such as boron carbide, titanium carbide, tungsten carbide, etc.) and the carbide supported low-cost high-efficiency catalyst (such as MnO) for rechargeable zinc-air battery according to claim 12，Co3O4Etc.) non-carbon based air electrode material and air electrode containing the same, and applying the same to zinc-air battery, characterized in that: when the battery is assembled, the anode material is titanium mesh, nickel mesh, stainless steel mesh, foamed nickel and the like coated with the air electrode material, and the electrolyte is 1-8M KOH and 0.1-0.5M Zn (CH)3COO)2The cathode material is a zinc sheet with the thickness of 0.1-1 mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111900388A (en) * | 2020-05-26 | 2020-11-06 | 北京理工大学 | Zinc ion battery negative electrode material, preparation and application thereof |
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| CN103730665A (en) * | 2012-10-15 | 2014-04-16 | 丰田自动车株式会社 | Air cathode for air batteries and air battery |
| CN105449233A (en) * | 2015-11-24 | 2016-03-30 | 北京工业大学 | Air electrode catalyst of rechargeable type zinc-air battery and preparation method of air electrode catalyst |
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- 2018-10-17 CN CN201811213401.XA patent/CN111063895A/en active Pending
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| CN103730665A (en) * | 2012-10-15 | 2014-04-16 | 丰田自动车株式会社 | Air cathode for air batteries and air battery |
| CN105449233A (en) * | 2015-11-24 | 2016-03-30 | 北京工业大学 | Air electrode catalyst of rechargeable type zinc-air battery and preparation method of air electrode catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111900388A (en) * | 2020-05-26 | 2020-11-06 | 北京理工大学 | Zinc ion battery negative electrode material, preparation and application thereof |
| CN111900388B (en) * | 2020-05-26 | 2021-12-07 | 北京理工大学 | Zinc ion battery negative electrode material, preparation and application thereof |
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Application publication date: 20200424 |