CN107732261A - A kind of boron carbide carried noble metal Oxygen Electrode Material for chargeable lithium-air battery - Google Patents
A kind of boron carbide carried noble metal Oxygen Electrode Material for chargeable lithium-air battery Download PDFInfo
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- CN107732261A CN107732261A CN201711101025.0A CN201711101025A CN107732261A CN 107732261 A CN107732261 A CN 107732261A CN 201711101025 A CN201711101025 A CN 201711101025A CN 107732261 A CN107732261 A CN 107732261A
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- oxygen electrode
- lithium
- air battery
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- electrode 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
- 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
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- 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
- Y02E60/10—Energy storage using batteries
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- Chemical Kinetics & Catalysis (AREA)
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- Hybrid Cells (AREA)
- Inert Electrodes (AREA)
Abstract
The present invention relates to the Oxygen Electrode Material of lithium-air battery, be specifically exactly a kind of noble-metal-supported that catalytic activity is high on stable boron carbide, being prepared as Oxygen Electrode Material turns into oxygen electrode, and is applied to chargeable lithium-air battery.Its preparation process includes：(1) Oxygen Electrode Material of boron carbide carried noble metal is prepared using hydrothermal synthesis reaction；(2) Oxygen Electrode Material of preparation and binding agent are mixed with oxygen electrode slurry；(3) slurry is coated uniformly in oxygen electrode collector substrate, oxygen electrode is obtained after drying；(4) lithium-air battery is assembled in glove box；(5) chemical property and charge-discharge performance of battery are tested respectively using electrochemical workstation and battery charging and discharging test system.The present invention is simple to operate, and prepared Oxygen Electrode Material is to have the boron carbide carried noble metal of high activity and high stability concurrently.This Oxygen Electrode Material can improve the charge-discharge performance and specific capacity of chargeable lithium-air battery.
Description
(1) technical field
The present invention relates to lithium-air battery Oxygen Electrode Material, specifically exactly a kind of noble metal that catalytic activity is high is born
It is loaded on stable boron carbide, as the Oxygen Electrode Material of chargeable lithium-air battery, prepares as the material is included
Oxygen electrode, and it is applied to chargeable lithium-air battery.
(2) background technology
The fast development of current electric car and portable electrical appliance proposes higher and higher performance requirement to electrochmical power source,
It is required that electrochmical power source has the characteristics that higher than energy, specific power is high, charge-discharge performance is good, security is good.Possess superelevation reason
By energy density, and lower cost for material, environment-friendly lithium-air battery turn into most promising high specific energy of new generation and quantified
Learn one of power supply.Its anode reactant is oxygen, in an atmosphere aboundresources, and procurement cost is extremely cheap, can effectively drop
The cost of low battery.Based on Li2O2Generation and decomposition reaction, the theoretical energy density of lithium-air battery may be up to 3600Wh/
Kg, its actual entire package energy density are expected to reach 600Wh/kg, and the provided energy that burnt close to gasoline in internal combustion engine is close
Spend 700Wh/kg.Just because of the significant advantage in energy density, lithium-air battery is considered as that can substitute conventional lithium ion
The energy-storage system of future generation of battery.
Many R＆D institutions of the world have all carried out correlative study at present.It is " Battery as IBM is carrying out a key name
500 Proiect " the research for scheduling to last the several years, it is desirable to make the course continuation mileage of electric automobile single charge reach 500 miles；Toyota
" battery research department " was also set up in 2008, is actively pushing forward the research of lithium-air battery；In addition AUS research is real
Test the research institution such as room and the laboratory of USDOE subordinate and also successively carry out correlative study.
The oxygen electrode of lithium-air battery is divided into carbon electrode and non-carbon electrode.The oxygen electrode deficient in stability of carbon material, can lead
Send a telegraph the capacity attenuation in pond and limit the cycle performance of battery.The discharging product Li in discharge process2O2Easily occur with carbon secondary anti-
Li should be generated2CO3, electrolyte can also generate Li in discharge process2CO3With the carboxylate of lithium.In charging process, Li2CO3And lithium
Carboxylate oxidation Decomposition can occur, when voltage is higher than 3.5V carbon electrode can also occur electrochemical oxidation generation CO2, will soon
The charging voltage of battery is raised rapidly, the decomposition of electrolyte and carbon positive pole can be further speeded up in this case, formed pernicious
Circulation.Therefore, the research and development of high activity, the Oxygen Electrode Material of high stability become most important.
(3) content of the invention
It is an object of the invention to provide a kind of oxygen of boron carbide carried noble metal for chargeable lithium-air battery electricity
The preparation of pole material, and by its application and chargeable lithium-air battery.
It is first in a kind of preparation method of the lithium-air battery Oxygen Electrode Material of boron carbide carried noble metal provided by the invention
First noble metal (can be Pt, Ru, Au, Rh etc.) chloride, boron carbide, sodium citrate, solvent are mixed and carried out with certain proportion
Stirring, in whipping process, mixing time is 10~15 hours, and the temperature of stirring is 50~70 DEG C, rotating speed is 300~
600rpm, adjust pH value with 5~10 (wt) %KOH ethylene glycol solution so that pH value is 9~14.Then by precursor solution
It is transferred in hydrothermal reaction kettle, puts in an oven, carry out hydrothermal synthesis reaction.
In a kind of preparation method of the lithium-air battery Oxygen Electrode Material of boron carbide carried noble metal provided by the invention, adopt
Catalyst powder is prepared with hydrothermal synthesis method, heating-up temperature is 120~180 DEG C, is heated 10~15 hours.PH is adjusted after cooling
Value.
In a kind of preparation method of the lithium-air battery Oxygen Electrode Material of boron carbide carried noble metal provided by the invention, adjust
Save the salpeter solution that pH value uses 5~15% so that the pH value of solution is 3~5, then spent glycol, deionized water and isopropyl
Alcohol washs, filters, centrifuges, is dried to obtain powder.
A kind of noble-metal-supported that catalytic activity is high provided by the invention is on stable boron carbide, as can fill
The Oxygen Electrode Material of electric lithium-air battery, and preparation turns into the oxygen electrode comprising the material, specific preparation method is：By catalyst
The ground and mixed in mortar uniformly obtains slurry with 6: 4~9: 1 ratio for powder and binding agent, then electric with oxygen is coated uniformly on
Pole collector substrate surface, dried 6~10 hours at 60~90 DEG C in vacuum drying chamber, that is, obtain oxygen electrode.
In a kind of lithium-air battery Oxygen Electrode Material preparation method of boron carbide carried noble metal provided by the invention, prepare
During anode sizing agent, the binding agent used is the organic binder bond such as PTFE, PVDF.
On a kind of boron carbide provided by the invention in the preparation method of the lithium air battery positive electrode catalyst of carried noble metal,
When preparing positive electrode, the oxygen electrode collector substrate used can be carbon paper, nickel screen, stainless (steel) wire, nickel foam etc..
On a kind of boron carbide provided by the invention the preparation method of the lithium-air battery Oxygen Electrode Material of carried noble metal with
In, concrete application shows as assembling buckle type rechargeable lithium-air battery.Lithium-air battery is assembled in the hand full of argon gas
Carried out in casing, H in glove box2O and O2Content is both less than 0.1ppm, specific battery pack turn into anode cover, positive plate, electrolyte,
Barrier film, pad, shell fragment, lithium piece (negative pole) and negative electrode casing.
A kind of preparation method of the lithium-air battery Oxygen Electrode Material of boron carbide carried noble metal provided by the invention is with answering
In, during assembled battery, the lithium piece diameter used can be 8~12mm.
A kind of preparation method of the lithium-air battery Oxygen Electrode Material of boron carbide carried noble metal provided by the invention is with answering
In, during assembled battery, lithium salts can be double trifluoromethanesulfonimide lithiums (LiTFSI) in the electrolyte used, trifluoromethanesulfonic acid
Lithium (LiTf), LiNO3, LiClO4Deng solvent can be glycol dimethyl ether (DME), tetraethyleneglycol dimethyl ether (TEGDME), diformazan
Base sulfoxide (DMSO) etc., concentration can be 0.5~2M.
On a kind of boron carbide provided by the invention the preparation method of the lithium-air battery Oxygen Electrode Material of carried noble metal with
The barrier film used in, during assembled battery is commercialization glass fiber filter paper, a diameter of 10~20mm of barrier film.
A kind of preparation method of the lithium-air battery Oxygen Electrode Material of boron carbide carried noble metal provided by the invention is with answering
In, when testing battery performance, the test device used is electrochemical workstation and battery charging and discharging test system, using electricity
Chem workstation tests the AC impedance of battery, charge-discharge performance and circulation using battery charging and discharging test system and test battery
Performance.
(4) illustrate
Fig. 1 Ru/B4Transmission electron microscope (TEM) figure of C positive electrode material
AC impedance before the test of Fig. 2 lithium-air batteries
Fig. 3 Oxygen Electrode Materials and the complete charge and discharge electrograph of lithium-air battery that binding agent ratio is 9: 1
Fig. 4 Oxygen Electrode Materials and binding agent ratio are the capacity circulating performance maps such as 9: 1 lithium-air battery
Fig. 5 Oxygen Electrode Materials and binding agent ratio are ESEM (SEM) figure of 9: 1 lithium-air battery discharging product
Following examples will be further described to the present invention, but not thereby limiting the invention.
Embodiment 1
Precious metal chloride, boron carbide, sodium citrate, solvent are mixed and are stirred with certain proportion, mixing time
For 10~15 hours, the temperature of stirring was 50~70 DEG C, and rotating speed is 300~600rpm, with 5~10 (wt) %KOH ethylene glycol
Solution adjusts pH value so that pH value is 9~14.It is then transferred into hydrothermal reaction kettle, puts in an oven, add at 120~180 DEG C
Heat 10~15 hours, after cooling add 5~15% salpeter solution cause solution pH value be 3~5, then spent glycol,
Deionized water and isopropanol wash, filter, centrifuge, are dried to obtain powder.The TEM figures of gained powder are shown in Fig. 1.
Embodiment 2
When preparing oxygen electrode slurry, the ratio of powder and binding agent is 6: 4~9: 1 for experiment.It is a certain amount of with weighing first
Ru/B4Then C powders add a certain amount of PVDF or PTFE binding agents by the way of being added dropwise, ground in mortar in mortar
Mill makes binding agent be sufficiently mixed with powder, obtains anode sizing agent.A diameter of 8~12mm nickel foam is cut with slicer, by oxygen
Electrode slurry is coated uniformly on oxygen electrode collector substrate surface, and oxygen electrode collector substrate can be carbon paper, nickel screen, stainless steel
Net, nickel foam etc..Then dried 6~10 hours at 60~90 DEG C in vacuum drying chamber, that is, obtain chargeable lithium-air battery
Oxygen electrode.Assembled battery is carried out in the glove box full of argon gas, positive electrode is carbon paper, the nickel for scribbling Oxygen Electrode Material
Net, stainless (steel) wire, nickel foam etc..Barrier film is glass fiber filter paper.Electrolyte is 0.5~2M double trifluoromethanesulfonimide lithiums
Or trifluoromethanesulfonic acid lithium (LiTf) or LiNO (LiTFSI)3Or LiClO4Etc. being dissolved in glycol dimethyl ether (DME) or tetrem two
In diethylene glycol dimethyl ether (TEGDME) or dimethyl sulfoxide (DMSO) (DMSO) equal solvent.Negative material is lithium piece, a diameter of 8~12mm.Specifically
Experimental procedure is：Put well first with foraminate anode cover, then put the carbon paper for scribbling Oxygen Electrode Material, nickel screen, stainless (steel) wire, bubble
Foam nickel etc., is then placed above barrier film in oxygen electrode, on barrier film be added dropwise electrolyte soak barrier film, finally put successively lithium piece,
Pad, shell fragment, negative electrode casing.The battery assembled is subjected to performance test.When carrying out battery testing, the friendship of battery is tested first
Flow impedance, see Fig. 2.Then charge-discharge test is carried out to battery, specific experiment result is shown in Fig. 3.
Embodiment 3
When preparing oxygen electrode slurry, the ratio of powder and binding agent is 6: 4~9: 1 for experiment.In the gloves full of argon gas
Carry out assembled battery in case, Oxygen Electrode Material is to scribble the carbon paper of Oxygen Electrode Material, nickel screen, stainless (steel) wire, nickel foam etc., barrier film
For glass fiber filter paper, double trifluoromethanesulfonimide lithiums (LiTFSI) or the trifluoromethanesulfonic acid lithium that electrolyte is 0.5~2M
Or LiNO (LiTf)3Or LiClO4Etc. being dissolved in glycol dimethyl ether (DME) or tetraethyleneglycol dimethyl ether (TEGDME) or diformazan
In base sulfoxide (DMSO) equal solvent.Negative material is lithium piece, a diameter of 8~12mm.Then charge-discharge cycle is carried out to battery
It can test, charging and discharging capacity is fixed as 300mAh/g, carries out cycle performance test, sees Fig. 4.
Embodiment 4
The chargeable lithium-air battery tested is dismantled in glove box, oxygen electrode therein is taken out, uses solvent
Cleaned 3~5 times in ampoule, solvent can be glycol dimethyl ether (DME), tetraethyleneglycol dimethyl ether (TEGDME), acetonitrile etc..
Oxygen electrode is placed in glove box and dried, using the pattern of ESEM (SEM) observation discharging product after drying, sees Fig. 5.
Claims (5)
- A kind of 1. boron carbide carried noble metal Oxygen Electrode Material for chargeable lithium-air battery, it is characterised in that：Will catalysis The high noble-metal-supported of activity as the Oxygen Electrode Material of chargeable lithium-air battery, and is made on stable boron carbide It is standby to turn into the oxygen electrode comprising the material, and it is applied to chargeable lithium-air battery.
- 2. a kind of boron carbide carried noble metal Oxygen Electrode Material for chargeable lithium-air battery described in claim 1 and comprising The preparation method of the oxygen electrode of the material, it is characterised in that：Oxygen Electrode Material powder is prepared, raw material use precious metal element Chloride, sodium citrate, the boron carbide of (can be Pt, Ru, Au, Rh etc.), using hydrothermal synthesis reaction method, solvent uses ethylene glycol And isopropanol.Precious metal chloride, boron carbide, sodium citrate, solvent are mixed and are stirred with certain proportion first, is stirred Time is 10~15 hours, and temperature is 50~70 DEG C, and rotating speed is 300~600rpm.With the second two containing 5~10 (wt) %KOH Alcoholic solution adjusts pH value so that pH value is 9~14.Then precursor solution is transferred in hydrothermal reaction kettle, put in an oven, Being heated at 120~180 DEG C 10~15 hours, the salpeter solution for instilling 5~15% after cooling make it that the pH value of solution is 3~5, Then spent glycol, deionized water and isopropanol wash, filter, centrifuge, are dried to obtain powder.
- 3. a kind of boron carbide carried noble metal Oxygen Electrode Material for chargeable lithium-air battery described in claim 1 and comprising The preparation method of the oxygen electrode of the material, it is characterised in that：(1) when preparing oxygen electrode slurry, the ratio of positive pole powder and binding agent is 6: 4~9: 1.(2) positive pole powder and binding agent ground and mixed are uniformly prepared into slurry in mortar, slurry is coated in oxygen electrode collection Fluid substrate surface, oxygen electrode collector substrate can be carbon paper, nickel screen, stainless (steel) wire, nickel foam etc., 60 in vacuum drying chamber Dried 6~10 hours at~90 DEG C, that is, obtain oxygen electrode.
- 4. according to a kind of boron carbide carried noble metal Oxygen Electrode Material for chargeable lithium-air battery described in claim 3 and The preparation method of oxygen electrode comprising the material, it is characterised in that：The binding agent used in the step (1) is PVDF, PTFE Deng organic binder bond.
- 5. a kind of boron carbide carried noble metal Oxygen Electrode Material for chargeable lithium-air battery described in claim 1 and comprising The oxygen electrode of the material, and it is applied to lithium-air battery, it is characterised in that：Assembling can in the glove box full of argon gas Charge lithium-air battery, just extremely carried noble metal/carbon paper of boron carbide Oxygen Electrode Material, nickel screen, stainless (steel) wire, nickel foam Deng a diameter of 8~12mm.Barrier film is glass fiber filter paper, a diameter of 10~20mm.Lithium salts can be double fluoroforms in electrolyte Sulfimide lithium (LiTFSI), trifluoromethanesulfonic acid lithium (LiTf), LiNO3, LiClO4Deng solvent can be glycol dimethyl ether (DME), tetraethyleneglycol dimethyl ether (TEGDME), dimethyl sulfoxide (DMSO) (DMSO) etc., concentration can be 0.5~2M.Negative material is lithium Piece, a diameter of 8~12mm.
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| CN201711101025.0A CN107732261A (en) | 2017-11-08 | 2017-11-08 | A kind of boron carbide carried noble metal Oxygen Electrode Material for chargeable lithium-air battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112067672A (en) * | 2020-09-11 | 2020-12-11 | 昆山宝创新能源科技有限公司 | Method for testing specific capacity of pre-lithiated lithium powder and application thereof |
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2017
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Patent Citations (4)
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| CN102088093A (en) * | 2011-01-04 | 2011-06-08 | 武汉理工大学 | Fuel cell catalyst taking conductive ceramic boron carbide as supporter and preparation method thereof |
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| CN112067672A (en) * | 2020-09-11 | 2020-12-11 | 昆山宝创新能源科技有限公司 | Method for testing specific capacity of pre-lithiated lithium powder and application thereof |
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Application publication date: 20180223 |