CN107785590A - A kind of high rate capability air electrode material and its application - Google Patents
A kind of high rate capability air electrode material and its application Download PDFInfo
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- CN107785590A CN107785590A CN201610734164.6A CN201610734164A CN107785590A CN 107785590 A CN107785590 A CN 107785590A CN 201610734164 A CN201610734164 A CN 201610734164A CN 107785590 A CN107785590 A CN 107785590A
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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
- H01M4/8605—Porous electrodes
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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
- H01M12/04—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
- H01M12/06—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type with one metallic and one gaseous electrode
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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
- H01M4/9008—Organic or organo-metallic compounds
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Abstract
The invention discloses a kind of high rate capability air electrode material and its application.The high rate capability air electrode material of the present invention includes conductive agent, binding agent and fluorine carbon activity agent.The high rate capability air electrode is by the way that by electrode material coating, baking is made on a current collector.There is the high rate capability air electrode prepared using the inventive method excellent high rate performance, active pore structure therein can ensure the high power discharge for making discharging product grow, realize lithium-air battery in its pore interior during high-multiplying power discharge.
Description
Technical field
The present invention relates to electrochemical energy storage field, in particular it relates to a kind of high rate capability air electrode material and its should
With.
Background technology
Lithium-air battery is the emerging battery system (3505 watt-hours/kilogram) for having highest theoretical energy density, by industry
Unanimously think it will is only selection of the substitution lithium ion battery as following main flow energy-storage system.But it is limited by it and is being circulated throughout
The irreversible side reaction at positive and negative electrode end in journey, the cycle efficieny of lithium-air battery, cycle life and power output are still difficult
To meet further practical application request, especially battery high rate performance poor in discharge process greatly governs lithium
The power output of air cell system.
For the air cathode in lithium-air battery, existing literature work sutdy concentrates on the modification of cyclical stability substantially
On.Adjusted by using liquid/solid state catalyst or material microstructure, can be 500-1000 MAhs/g of restriction capacity region
Interior maintenance lithium-air battery charge and discharge cycles more than 100 weeks.Only a few studies are being put by electrode material and structure design
Certain lifting is obtained in terms of electric high rate performance.Wherein, can be in the electricity of 3000 milliamperes/gram by using thin electrolyte material electrode
Under current density, discharge capacity is set to reach 1500 MAhs/g.But above discharge capacity apart from air electrode theoretical capacity according to
It is so far apart.
Described in summary, the preparation method of existing lithium air cathode material can not make a breakthrough in terms of high rate performance modification,
Large Copacity electric discharge almost blank is particularly realized under the conditions of high rate cyclic.Therefore, this area there is an urgent need to develop one kind can
There is the lithium air cathode material and its preparation technology of high rate capability and high discharge capacity simultaneously.
The content of the invention
It is an object of the invention to provide a kind of air electrode material and preparation method thereof.
The first aspect of the present invention provides a kind of air electrode material, and the high rate capability air electrode material includes
Conductive agent, binding agent and fluorine carbon activity agent.
Air electrode material as described in the first aspect of the invention, wherein, described fluorine carbon activity agent is with Rf-L-X
The compound of structural formula：
In formula,
RfFor the C4-C20 carbochains substituted completely or partially, wherein described substitution refers to that fluorine atom substitutes；
X is polar group, is selected from the group：-OH、-SH、-CN、-NO3、-CHO、-COOH、-SO3H, C1-C6 alkoxies, C3-
C6 miscellaneous alkyls；
L is divalent linker, the alkylidene of the alkylidene selected from C0-C6, preferably C1-C3.
In another preference, described RfFor the C5-C15 carbochains of part fluoro.
In another preference, described RfFor the C6-C10 carbochains of part fluoro.
In another preference, described RfFor the C5-C15 carbochains of complete fluoro.
In another preference, described RfFor the C6-C10 carbochains of complete fluoro.
In another preference, described activating agent includes the following group：
In another preference, heretofore described fluorocarbon surfactant includes：The conventional material in this area, or use
Prepared by conventional method, or be commercially available from market, or its combination.
In another preference, the conductive agent include special close highly conductive carbon black, Ketjen black, acetylene black, CNT and
Other conventional conductive agents or its combination.
In another preference, the binding agent include polytetrafluoroethylene (PTFE), Kynoar and other conventional binders or
It is combined.
In another preference, the weight ratio of the conductive agent, binding agent and fluorine carbon activity agent is 40~80：10~20：
10~40.
In another preference, the conductive agent load capacity is 0.01~0.1 milli gram/cm.
In another preference, described conductive agent load capacity is 0.04~0.05 milli gram/cm.
In another preference, the collector is selected from the group：Nickel foam, carbon paper.
In another preference, the collector is selected from the group：Nickel foam.
In another preference, electric discharge of the manufactured air electrode under the conventional current density of 500 milliamperes/gram is held
Measure as 16000 MAhs/g；Discharge capacity under the current density of 5000 milliamperes/gram is 1800 MAhs/g.
The second aspect of the present invention provides a kind of high magnification air electrode preparation method, and step is as follows：
(1) binding agent is stirred in solvent and is pre-dissolved acquisition binder solution, binder solution concentration is no more than mass ratio
30%；
(2) acquisition electrode material will be stirred in solvent in (1) of conductive agent, binder solution and the agent of fluorine carbon activity
Slurry；
(3) electrode material slurry is sprayed in collector one side, low-temperature prewarming solvent flashing by spray gun, obtained standby
Electrode.
In another preference, described solvent is selected from the group：Water, 1-METHYLPYRROLIDONE, N,N-dimethylformamide,
DMA, dimethyl sulfoxide (DMSO), or its combination.
In another preference, the solvent is water.
In another preference, the stirring is magnetic agitation.
In another preference, the time of stirring is 1~5 hour in the step (1) and/or (2), it is therefore preferable to 2~3
Hour.
In another preference, binder solution concentration is 5~30% in the step (1), it is therefore preferable to 10%.
In another preference, the low-temperature prewarming temperature is 80~140 DEG C, is more preferably 100~120 DEG C.Another
In preference, described baking time is 1~20h, is more preferably 3~15h.
In another preference, the baking is carried out under vacuum environment or inert gas shielding.
Air electrode material as described in the present invention, which is mainly used in, prepares air electrode or lithium-air battery.
Brief description of the drawings
Fig. 1 is the rate discharge curves variation diagram of the gained air electrode 1 of embodiment 1.
Embodiment
The present inventor have unexpectedly discovered that a kind of high rate capability air electrode material first by depth studying extensively
Material, the air electrode prepared using the air electrode material have excellent high rate performance, active pore structure therein can
Ensure to make discharging product in the growth of its pore interior during high-multiplying power discharge, realize the high power discharge of lithium-air battery.
On this basis, the present invention is completed.
Term
As used herein, term " agent of fluorine carbon activity " or " fluorocarbon surfactant " are used interchangeably, and are referred to hydrocarbon surface and are lived
Hydrogen atom in the hydrocarbon chain of property agent is completely or partially replaced by fluorine atoms, i.e., fluorocarbon chain instead of hydrocarbon chain as nonpolar base
The surfactant of group.
In a particular embodiment, the fluorine carbon activity agent used in the present invention is with RfThe compound of-L-X structural formulas,
In formula, RfFor the C4-C20 carbochains substituted completely or partially, wherein described substitution refers to that fluorine atom substitutes；X is polar group,
It is selected from the group：-OH、-SH、-CN、-NO3、-CHO、-COOH、-SO3H, C1-C6 alkoxies, C3-C6 miscellaneous alkyls；L connects for divalence
Group, the alkylidene of the alkylidene selected from C0-C6, preferably C1-C3.
In a particular embodiment, described RfFor the C5-C15 carbochains of part fluoro；Preferably, described RfFor portion
Divide the C6-C10 carbochains of fluoro.In a particular embodiment, described RfCan also be the C5-C15 carbochains of complete fluoro；It is excellent
Selection of land, described RfFor the C6-C10 carbochains of complete fluoro.
In a preferred embodiment, described activating agent includes the following group：
Those skilled in the art know that fluorocarbon surfactant of the present invention can include：The conventional material in this area
Material, or prepared with conventional method, or be commercially available from market, or its combination.
In the present invention, term " air electrode material ", " lithium air cathode material " have identical implication, and the material is by collecting
Fluid and air electrode material of main part coated on collector one side are combined, wherein, described air electrode main body material
Material includes conductive agent, binding agent and fluorine carbon activity agent.
Activating agent used in the present invention is fluorine carbon activity agent, and its source includes (but being not limited to)：The conventional material in this area
Material, or prepared with conventional method, or be commercially available from market, or its combination.
Conductive agent load capacity used in the present invention is 0.04~0.05 milli gram/cm, and its source includes (but and unlimited
In)：Special close highly conductive carbon black (Super-P), Ketjen black, acetylene black, CNT and other conventional conductive agents or its combination.
Binding agent used in the present invention includes (but being not limited to)：Polytetrafluoroethylene (PTFE), Kynoar and other conventional adhesives
Agent or its combination.
Wherein, the weight ratio of conductive agent, binding agent and fluorine carbon activity agent is 40~80：10~20：10~40.
Characterized by small angle X-ray diffraction, inventor has found that in discharge process air electrode material of the invention is made
Lithium-air battery main discharge product, i.e. lithium peroxide can be grown in the electrode hole of fluorine-containing carbon activity agent so that electricity
Pole hole utilization rate is greatly improved, and also just because of this, its discharge capacity is much larger than the air electrode of not fluorine-containing carbon activity agent.
In discharge process, air electrode made of the electrode material with fluorine carbon activity agent of the invention can be in 500 millis
Peace/gram conventional current density be issued to 16000 MAhs/g of superelevation discharge capacity；Even if current density is promoted to
5000 milliamperes/gram, its discharge capacity can still maintain 1800 MAhs/g.
Preparation method
The present invention provides the preparation method of air electrode, including step：
(1) binding agent is stirred in solvent and is pre-dissolved acquisition binder solution；
(2) acquisition electrode material will be stirred in solvent in (1) of conductive agent, binder solution and the agent of fluorine carbon activity
Slurry；
(3) electrode material slurry is sprayed in collector one side, low-temperature prewarming solvent flashing by spray gun, obtains electricity
Pole.
In a particular embodiment, described solvent is selected from the group：Water, 1-METHYLPYRROLIDONE, N, N- dimethyl methyls
Acid amides, DMA, dimethyl sulfoxide (DMSO), or its combination；Preferably, the solvent is water.
In a particular embodiment, the preparation method of air electrode of the invention uses magnetic agitation.
In a preferred embodiment, the time of the step (1) and/or (2) middle stirring is 1~5 hour, it is therefore preferable to
2~3 hours.
In a preferred embodiment, binder solution concentration is 5~30% in the step (1), it is therefore preferable to 10%.
In another preferred embodiment, the low-temperature prewarming temperature is 80~140 DEG C, is more preferably 100~120
℃.In a preferred embodiment, described baking time is 1~20h, is more preferably 3~15h.
In a preferred embodiment, the low-temperature prewarming is carried out under vacuum environment or inert gas shielding.
The main advantages of the present invention
In discharge process, lithium-air battery main discharge product, i.e. lithium peroxide can be grown on the electricity of fluorine-containing carbon activity agent
In the hole of pole so that electrode hole utilization rate is greatly improved.There is an advantage in that：
(1) under conventional current density, lithium-air battery discharge capacity is far above air electricity prepared by other Existing methods
Pole.
(2) extremely excellent discharge-rate performance, can guarantee that and higher discharge capacity is issued in high current density.
(3) the succinct actual effect of the synthetic method of high rate capability air electrode, large batch of electrode can disposably be located
Reason, has huge application potential.
The features described above that the present invention mentions, or the feature that embodiment is mentioned can be in any combination.Disclosed in this case specification
All features can be used in combination with any combinations thing form, each feature disclosed in specification, can with it is any be provided it is identical,
The alternative characteristics substitution of impartial or similar purpose.Therefore except there is special instruction, disclosed feature is only impartial or similar spy
The general example of sign.
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.The experimental method of unreceipted actual conditions in the following example, generally according to conventional strip
Part or according to the condition proposed by manufacturer.Unless otherwise indicated, otherwise percentage and number are calculated by weight.
Unless otherwise defined, anticipated known to all specialties used in text and scientific words and one skilled in the art
Justice is identical.In addition, any method similar or impartial to described content and material all can be applied in the inventive method.Wen Zhong
Described preferable implementation only presents a demonstration with material to be used.
Embodiment 1
The preparation of high rate capability air electrode 1
A, the polytetrafluoroethylene (PTFE) that mass ratio is 6% is dissolved in aqueous solvent, stirring 3 hours is mixed in magnetic stirring apparatus,
Obtain homogeneous solution；
B, in mass ratio 58:11:31 are stirred conductive agent：Polytetrafluoroethylene (PTFE)：Fluorine carbon activity agentFS-
3100 (Du PontsTM), water is added in the mixture and is placed in mixing stirring 3 hours in magnetic stirring apparatus, obtains uniform sizing material；
C, the slurry in step b is sprayed in nickel foam one side by spray gun, with 120 DEG C of bakings 12 in vacuum environment
Hour；
D, the standby pole piece prepared in step c is cut into a diameter of 14 millimeters of disk as having high rate capability air
The pole piece of electrode material；
Lithium perchlorate electrolyte with dimethyl sulfoxide (DMSO) (DMSO) for 0.1 mol/L of solvent is pressed to 140 microlitres of amount e,
Instill in Whatman GF/D fibreglass diaphragms, and with the air electrode pole piece obtained in d and to electrode metal lithium piece one
Rise and load CR2032 type button cell shells, be put into assembling in the glove box containing inert gas and obtain the electricity of air containing high rate capability
The lithium-air battery of pole 1.
As a result
In the case where current density is the multiplying power of 500 milliamperes/gram, to the lithium air of obtained air electrode containing high rate capability 1
Battery carries out the discharge test that stopping potential window is 2V, and discharge capacity reaches 16368.4 MAhs/g (tables 1).Other one
In kind multiplying power test, discharge capacity respectively reaches 10367.6,5195.4 and under 1000,2000 and 5000 milliamperes/gram
1802 MAhs/g (Fig. 1).
Embodiment 2
The preparation of high rate capability air electrode 2
Embodiment 1 is repeated, difference is：Conductive agent in stepb：Polyacrylonitrile：Fluorine carbon activity agent
FS-3100 (Du PontsTM) in mass ratio 66:22:12 mix.
Embodiment 3
The preparation of high rate capability air electricity 3
Embodiment 1 is repeated, difference is：Conductive agent in stepb：Polyacrylonitrile：Fluorine carbon activity agent
FS-3100 (Du PontsTM) in mass ratio 50:12:38 mix.
Comparative example 1
The preparation of regular air electrode 1
A, the polytetrafluoroethylene (PTFE) that mass ratio is 6% is dissolved in aqueous solvent, stirring 3 hours is mixed in magnetic stirring apparatus,
Obtain homogeneous solution；
B, in mass ratio 85:15 are stirred conductive agent：Polytetrafluoroethylene (PTFE), water is added in the mixture and is placed in magnetic force and stirs
Mix and stirring 3 hours is mixed in device, obtain uniform sizing material；
C, the slurry in step b is sprayed in nickel foam one side by spray gun, with 120 DEG C of bakings 12 in vacuum environment
Hour；
D, the standby pole piece prepared in step c is cut into a diameter of 14 millimeters of disk as having regular air electrode material
The pole piece of material；
Lithium perchlorate electrolyte with dimethyl sulfoxide (DMSO) (DMSO) for 0.1 mol/L of solvent is pressed to 140 microlitres of amount e,
Instill in Whatman GF/D fibreglass diaphragms, and with the air electrode pole piece obtained in d and to electrode metal lithium piece one
Rise and load CR2032 type button cell shells, be put into assembling in the glove box containing inert gas and obtain electrode containing regular air 1
Lithium-air battery.
As a result
In the case where current density is only the multiplying power of 100 milliamperes/gram, to the lithium-air battery of obtained regular air electrode 1
The discharge test that stopping potential window is 2V is carried out, discharge capacity reaches 804.6 MAhs/g (tables 1).It is in current density
Under the multiplying power of 500 milliamperes/gram, discharge capacity is almost 0 (0.0032 MAh/g).
Comparative example 2
The preparation of air electrode 1 with not fluorine-containing activating agent
A, the polytetrafluoroethylene (PTFE) that mass ratio is 6% is dissolved in aqueous solvent, stirring 3 hours is mixed in magnetic stirring apparatus,
Obtain homogeneous solution；
B, in mass ratio 58:11:31 are stirred conductive agent：Polytetrafluoroethylene (PTFE)：Polyvinylpyrrolidone (Polyvinyl
Pyrrolidone), water is added in the mixture to be placed in mixing stirring 3 hours in magnetic stirring apparatus, obtain uniform sizing material；
C, the slurry in step b is sprayed in nickel foam one side by spray gun, with 120 DEG C of bakings 12 in vacuum environment
Hour；
D, the standby pole piece prepared in step c is cut into a diameter of 14 millimeters of disk as having high rate capability air
The pole piece of electrode material；
Lithium perchlorate electrolyte with dimethyl sulfoxide (DMSO) (DMSO) for 0.1 mol/L of solvent is pressed to 140 microlitres of amount e,
Instill in Whatman GF/D fibreglass diaphragms, and with the air electrode pole piece obtained in d and to electrode metal lithium piece one
Rise and load CR2032 type button cell shells, be put into assembling in the glove box containing inert gas and obtain the electricity of air containing high rate capability
The lithium-air battery of pole 1.
Comparative example 3
The preparation of air electrode 1 with common fluorochemical
Comparative example 2 is repeated, difference is：Mixture and its ratio in stepb is mass ratio 50:12:38 lead
Electric agent：Polytetrafluoroethylene (PTFE)：1,2- (1,1,2,2- tetrafluoros ethyoxyl) ethane (1,2- (1,1,2,2-tetrafluoroethoxy)
ethane)。
As a result
It is empty to the lithium of air electrode 1 made from comparative example 2 and 3 in the case where current density is only the multiplying power of 100 milliamperes/gram
Pneumoelectric pond carries out the discharge test that stopping potential window is 2V, and discharge capacity only reaches 23.01 and 11.197 MAhs/g of (tables
1).In current density under the multiplying power of 500 milliamperes/gram, discharge capacity is almost 0 (0.142 and 0.1392 MAh/g).
The discharge capacity rate result of table 1
Pass through contrast, using high rate capability air electrode provided by the invention under conventional current density, electric discharge
Capacity is far above air electrode prepared by other Existing methods；Under high current density, it also can guarantee that the electric discharge for reaching higher is held
Amount.
All it is incorporated as referring in this application in all documents that the present invention refers to, it is independent just as each document
It is incorporated as with reference to such.In addition, it is to be understood that after the above-mentioned instruction content of the present invention has been read, those skilled in the art can
To be made various changes or modifications to the present invention, these equivalent form of values equally fall within the model that the application appended claims are limited
Enclose.
Claims (10)
1. a kind of air electrode material, it is characterised in that described air electrode material includes conductive agent, binding agent and fluorine carbon and lived
Property agent.
2. air electrode material as claimed in claim 1, it is characterised in that described fluorine carbon activity agent is with Rf- L-X is tied
The compound of structure formula：
In formula,
RfFor the C4-C20 carbochains substituted completely or partially, wherein described substitution refers to that fluorine atom substitutes；
X is polar group, is selected from the group：-OH、-SH、-CN、-NO3、-CHO、-COOH、-SO3H, C1-C6 alkoxies, C3-C6 are miscellaneous
Alkyl；
L is divalent linker, the alkylidene of the alkylidene selected from C0-C6, preferably C1-C3.
3. air electrode material as claimed in claim 1, it is characterised in that the conductive agent include special close highly conductive carbon black,
Ketjen black, acetylene black, CNT and other conventional conductive agents or its combination.
4. air electrode material as claimed in claim 1, it is characterised in that the binding agent includes polytetrafluoroethylene (PTFE), gathered partially
PVF and other conventional binders or its combination.
5. air electrode material as claimed in claim 1, it is characterised in that the conductive agent, binding agent and fluorine carbon activity agent
Weight ratio be 40~80：10~20：10~40.
6. air electrode material as claimed in claim 1, it is characterised in that the conductive agent load capacity is 0.01~0.1 milli
Gram/cm.
7. air electrode material as claimed in claim 1, it is characterised in that the collector is selected from the group：Nickel foam, carbon
Paper.
8. a kind of high magnification air electrode preparation method, it is characterised in that step is as follows：
(1) binding agent is stirred in solvent and is pre-dissolved acquisition binder solution, binder solution concentration is no more than mass ratio 30%；
(2) it will be stirred in solvent in (1) of conductive agent, binder solution and the agent of fluorine carbon activity and obtain electrode material slurry
Material；
(3) electrode material slurry is sprayed in collector one side, low-temperature prewarming solvent flashing by spray gun, obtains standby electricity
Pole.
9. method as claimed in claim 8, it is characterised in that described solvent is selected from the group：Water, 1-METHYLPYRROLIDONE,
DMF, DMA, dimethyl sulfoxide (DMSO), or its combination.
10. the air electrode material as any one of claim 1-7 should in air electrode or lithium-air battery is prepared
With.
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