CN108448115A - A kind of asymmetric skeleton structure of lithium metal battery cathode - Google Patents

A kind of asymmetric skeleton structure of lithium metal battery cathode Download PDF

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Publication number
CN108448115A
CN108448115A CN201810213944.5A CN201810213944A CN108448115A CN 108448115 A CN108448115 A CN 108448115A CN 201810213944 A CN201810213944 A CN 201810213944A CN 108448115 A CN108448115 A CN 108448115A
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skeleton
inconsistent
lithium metal
metal battery
lithium
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张强
张睿
程新兵
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Tsinghua University
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Tsinghua University
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

A kind of asymmetric skeleton structure of lithium metal battery cathode, belongs to lithium metal battery technical field.The skeleton structure has physicochemical property inconsistent in a thickness direction.By physicochemical properties such as the not quite identical material component of the skeleton structure, structure, electronic impedance, ionic resistance, electrolyte contact angle, molten lithium contact angle, specific surface area, pore size distribution, specific pore volume, porositys, it realizes in lithium metal battery charge and discharge process the intervention and guiding of the electronics conduction behavior in lithium ion transport behavior and skeleton structure between skeleton structure, and then realizes the accuracy controlling to lithium metal deposition position and dissolving position.Final high stability, the battery charging and discharging performance of high circulation efficiency for realizing the lithium metal battery negative material based on the skeleton structure under high magnification, high power capacity.

Description

A kind of asymmetric skeleton structure of lithium metal battery cathode
Technical field
The present invention relates to a kind of asymmetric skeleton structures of lithium metal battery cathode, belong to lithium metal battery technical field.
Background technology
The successful commercialization application of lithium ion battery has driven including smart mobile phone, wearable device, unmanned plane, electronic The high speed development of automobile and other industries.But in recent years, the energy density of lithium ion battery became closer to its theoretical limit, It is difficult to meet the needs of people and society higher and higher to energy-storage system.In numerous battery materials, lithium metal relies on its pole High theoretical specific capacity (3860mAh g-1) and minimum oxidation-reduction electrode current potential (- 3.040V vs. standard hydrogen electrodes) become Most promising next-generation secondary battery cathode material.
But lithium metal battery cannot achieve always large-scale commercial application, the main reason is that filling in lithium metal battery Electric process, i.e., easily growth forms dendritic Li dendrite, the appearance and growth of Li dendrite, one side in the deposition process of lithium metal Diaphragm may be pierced through to cause internal short-circuit of battery and then bring cell safety hidden danger, on the other hand also will increase metal in battery The problems such as irreversible consumption of lithium and electrolyte forms " dead lithium ", brings lithium an- ode material dusting, seriously reduces battery Cycle life.
To solve the growth question of Li dendrite, researcher proposes a variety of lithium anode (stones using framework material Black alkene skeleton, carbon fiber skeleton, foam copper skeleton, three-dimensional copper skeleton, glass fibre skeleton etc.).These framework materials can be with The lithium dendrite growth in lithium metal deposition process is effectively inhibited to a certain extent, and improves the cyclicity of lithium metal half-cell Energy.But under big multiplying power or large capacity cycling condition, the advantage of skeleton structure can not give full play of.For each section The consistent common conductive skeleton structure of physicochemical property, in big circulation, after deposited the lithium metal of a period of time, Lithium ion mobility to negative terminal surface in body phase electrolyte will be prior to skeleton structure outside deposition, and matrix porosity is electrolysed Lithium ion is almost depleted in matter and can not obtain the lithium ion of body phase electrolyte supplement in time so that the lithium metal in skeleton Deposition, which slows down, even to be stagnated, this ultimately causes lithium metal and is almost only deposited at the skeleton structure outer surface, and conducting matrix grain is made to lose Originally the effect of design.Similar problem also sees consistent common of other each section physicochemical properties such as insulation framework structure Skeleton structure.Therefore, design is a kind of having material component, structure, electronic impedance, ionic resistance, electrolyte in a thickness direction The not quite identical skeleton knot of the physicochemical properties such as contact angle, molten lithium contact angle, specific surface area, pore size distribution, specific pore volume, porosity Structure not only may be implemented to inhibit lithium metal growth and improve the effect of cathode cycle performance, can also be in big multiplying power, large capacity The effect of lithium metal battery cathode middle skeleton structure is given full play under charge status, realizes lithium metal deposition position and dissolving position The accuracy controlling set.
Invention content
The object of the present invention is to provide a kind of asymmetric skeleton structures of lithium metal battery cathode.This asymmetry skeleton knot Structure can realize lithium metal deposition position by the physicochemical property inconsistency on its thickness direction and dissolve the accurate tune of position Control.
Technical scheme is as follows:
A kind of asymmetric skeleton structure of lithium metal battery cathode, it is characterised in that:The skeleton structure has in thickness side Inconsistent physicochemical property upwards;Method is prepared the asymmetry skeleton structure one or more of as follows:
A. by physicochemical property it is different multiple material splicing or it is compound after skeleton structure is made;
B. same material is post-processed into the inconsistent rear formation skeleton structure of physicochemical property;
C. direct in-situ prepares the inconsistent material of physicochemical property and forms skeleton structure.
In technical scheme of the present invention, the inconsistent physicochemical property include material component is inconsistent, structure is inconsistent, Electronic impedance is inconsistent, ionic resistance is inconsistent, electrolyte contact angle is inconsistent, molten lithium contact angle is inconsistent, specific surface area It is inconsistent, one or more during pore size distribution is inconsistent, specific pore volume is inconsistent, porosity is inconsistent.
The asymmetry skeleton structure is made of one or both of conductive material and insulating materials.
Preferably, the conductive material is carbon black, fullerene, graphene, carbon nanotube, template carbon, macropore carbon, hollow carbon It is one or more in ball, activated carbon, carbon fiber, foamy carbon, copper, silver, gold, nickel, aluminium, iron, steel etc..The insulating materials is preferred For polyethylene, polypropylene, polyimides, polymer resin, polyacrylonitrile, polyvinyl chloride, polyethylene oxide, poly-methyl methacrylate Ester, polyether sulfone, Kynoar, Kynoar-hexafluoropropylene copolymer, cellulose acetate, polylactic acid, gathers oneself at polyaniline It is one or more in lactone, polytrimethylene carbonate, poly (lactic acid-glycolic acid), glass fibre.
The present invention compared with prior art, has the following advantages that and high-lighting effect:By this technology, prepare in thickness side Upwards with physicochemical property inconsistency framework material, by its not quite identical material component, structure, electronic impedance, The physicochemical properties such as ionic resistance, electrolyte contact angle, molten lithium contact angle, specific surface area, pore size distribution, specific pore volume, porosity, it is real Electronics conducts behavior in lithium ion transport behavior and skeleton structure between skeleton structure in present lithium metal battery charge and discharge process Intervention and guiding, and then realize to lithium metal deposition position and dissolving position accuracy controlling.Final realize is based on the skeleton The battery charging and discharging of high stability of the lithium metal battery negative material of structure under high magnification, high power capacity, high circulation efficiency Energy.
Specific implementation mode
A kind of asymmetric skeleton structure of lithium metal battery cathode provided by the invention, the skeleton structure have in thickness side Inconsistent physicochemical property upwards;One or more of as follows prepared by method for the asymmetry skeleton structure:
A. by physicochemical property it is different multiple material splicing or it is compound after skeleton structure is made;
B. same material is post-processed into the inconsistent rear formation skeleton structure of physicochemical property;
C. direct in-situ prepares the inconsistent material of physicochemical property and forms skeleton structure.
The inconsistent physicochemical property includes that material component is inconsistent, structure is inconsistent, electronic impedance is inconsistent, ion Impedance is inconsistent, electrolyte contact angle is inconsistent, molten lithium contact angle is inconsistent, specific surface area is inconsistent, pore size distribution is inconsistent, Specific pore volume is inconsistent one or more in inconsistent with porosity.
The asymmetry skeleton structure is made of one or both of conductive material and insulating materials.The conductive material Preferably carbon black, fullerene, graphene, carbon nanotube, template carbon, macropore carbon, hollow carbon balls, activated carbon, carbon fiber, foam It is one or more in carbon, copper, silver, gold, nickel, aluminium, iron and steel.The insulating materials is preferably polyethylene, polypropylene, polyamides Asia Amine, polyacrylonitrile, polyvinyl chloride, polyethylene oxide, polymethyl methacrylate, polyaniline, polyether sulfone, gathers partially polymer resin Vinyl fluoride, Kynoar-hexafluoropropylene copolymer, cellulose acetate, polylactic acid, polycaprolactone, polytrimethylene carbonate, It is one or more in poly (lactic acid-glycolic acid) and glass fibre.
The present invention is described further with reference to embodiment, but the scope of the present invention is not limited thereto.
Embodiment 1:It takes graphene powder to be put into tube furnace, is passed through H2With NH32:1 mixed gas, the constant temperature at 600 DEG C 30 minutes (or 60 minutes) carry out N doping reaction, and the nitrogen-doped graphene that N doping amount is atomic fraction 1% (or 2%) is made. By the graphene of the nitrogen-doped graphene of two kinds of itrogen content of getter with nitrogen dopeds of gained and non-nitrating, totally 3 groups of samples press carbon material and binder quality respectively Than 9:Kynoar binder is added in 1 ratio, then is separately added into the N-Methyl pyrrolidone dispersant of equivalent and is disperseed Stirring 24 hours obtains 3 groups of slurries.First on copper foil the nitrating graphite that one layer of itrogen content of getter with nitrogen doped is 2% is scratched using 100 μm of scrapers Alkene slurry scratches the nitrogen-doped graphene slurry that one layer of itrogen content of getter with nitrogen doped is 1% on gained coating using 100 μm of scrapers again after drying, Finally scratch the graphene slurry of one layer of non-nitrating after drying again using 100 μm of scrapers on gained coating.Gained pole piece dries It is the asymmetric bone of the lithium metal battery cathode in a thickness direction with different component and different molten lithium contact angles after dry Frame structure.The asymmetry skeleton structure is tested with common lithium piece as to electrode assembling half-cell, electrolyte is double three Methyl fluoride sulfimide lithium, 1,3- dioxolanes, ethylene glycol dimethyl ether solution.In 1.0mA cm-2Current density and 1.0mAh cm-2Under charge/discharge capacity, which can stablize 50 circle of cycle or more, and coulombic efficiency keeps 96%, passes through scanning electron microscope The interstitial space that the asymmetry skeleton structure can be made full use of when the visible removal lithium embedded in observation cathode pole piece section, realizes lithium metal The accurate regulation and control of deposition position and dissolving position.
Embodiment 2:It takes 3 batches of identical magnesium oxide templates for being loaded with Fe catalyst to be put into tube furnace, is passed through H2With CH4's 1:3 mixed gas, distinguish constant temperature 2 hours, 3 hours, 4 hours at 900 DEG C, to prepare the different carbon nanotube of 3 groups of length.Institute It obtains 3 groups of powder and the dilute hydrochloric acid dipping stirring of mass fraction 10% is respectively added to dissolve removal Fe catalyst and magnesia mould Plate, insoluble matter are carbon nanotube.3 groups of carbon nanotubes are filtered by suction filtration method on filter paper and drying respectively, obtain 3 The carbon nanotube paper that kind is made of different length carbon nanotube.3 kinds of carbon are received according to the sequence of length of carbon nanotube from short to long Mitron paper stacks from bottom to top, and is compressed to the combination cathode pole piece of thickness 1mm, obtains having different electricity in a thickness direction Sub- conductance, different porosities lithium metal battery cathode asymmetric skeleton structure.By the asymmetry skeleton structure and common lithium Piece matching assembling half-cell is tested, and electrolyte is bis trifluoromethyl sulfimide lithium, 1,3-dioxolane, glycol dinitrate Ethereal solution.In 1.0mA cm-2Current density and 1.0mAh cm-2Under charge/discharge capacity, which can stablize 40 circle of cycle or more, Coulombic efficiency keeps 94%, this can be made full use of not when observing the visible removal lithium embedded in cathode pole piece section by scanning electron microscope The interstitial space of symmetrical skeletal structure realizes lithium metal deposition position and dissolves the accurate regulation and control of position.
Embodiment 3:It is respectively 0.1mm and 0.5mm to prepare 2 apertures, and thickness is the foam copper of 1mm.By 2 foam coppers It is stacked in upper sequence by large aperture, and is compressed to the combination cathode pole piece that thickness is 1mm, had in a thickness direction Have different pore size, different porosities, Different Pore Structures lithium metal battery cathode asymmetric skeleton structure.By the asymmetry bone Frame structure matches assembling half-cell with common lithium piece and is tested, and electrolyte is bis trifluoromethyl sulfimide lithium, 1,3- dioxies Penta ring, ethylene glycol dimethyl ether solution.In 1.0mA cm-2Current density and 1.0mAh cm-2Under charge/discharge capacity, which can be steady Surely more than 80 circle of cycle, coulombic efficiency keeps 97%, and the visible removal lithium embedded in cathode pole piece section is observed by scanning electron microscope When can make full use of the interstitial space of the asymmetry skeleton structure, realize lithium metal deposition position and dissolve the accurate tune of position Control.
Embodiment 4:The carbon fiber paper that thickness is 500 μm is connected cathode to be put into electroplating pool, anode is silver plate, and makes sun Pole plate and cathode plate interval are only 2cm, and electroplate liquid is the silver nitrate aqueous solution that mass fraction is 1%, is passed through 100mA cm-2Electricity Electric current is plated, is electroplated 30 seconds.Strong-current electroplating in weak solution can make to obtain on porous carbon fiber non-uniform on thickness direction Silvering obtains the asymmetry with different component, the lithium metal battery cathode of different molten lithium contact angles in a thickness direction Skeleton structure.The asymmetry skeleton structure is matched assembling half-cell with common lithium piece to test, electrolyte is double fluoroforms Base sulfimide lithium, 1,3- dioxolanes, ethylene glycol dimethyl ether solution.In 1.0mA cm-2Current density and 1.0mAh cm-2It fills Under discharge capacity, which can stablize 70 circle of cycle or more, and coulombic efficiency keeps 96%, be observed by scanning electron microscope negative The interstitial space that the asymmetry skeleton structure can be made full use of when the visible removal lithium embedded in pole pole piece section realizes lithium metal deposition position Set and dissolve the accurate regulation and control of position.
Embodiment 5:Using zinc oxide target as target source, by the all-glass paper of 1 1mm thickness to a wherein face magnetron sputtering oxygen Change Zinc material, obtains the all-glass paper of uneven coating zinc oxide on thickness direction, front Zinc oxide coating thickness is about 100nm, and its back side does not have visible Zinc oxide coating.Obtain that there is different component, different electrolyte contacts in a thickness direction Angle, different lithium ion conductance lithium metal battery cathode asymmetric skeleton structure.By the asymmetry skeleton structure and common lithium Piece matching assembling half-cell is tested, and electrolyte is bis trifluoromethyl sulfimide lithium, 1,3-dioxolane, glycol dinitrate Ethereal solution.In 1.0mA cm-2Current density and 1.0mAh cm-2Under charge/discharge capacity, the battery can stablize cycle 150 circle with On, coulombic efficiency keeps 97%, can be made full use of when observing the visible removal lithium embedded in cathode pole piece section by scanning electron microscope The interstitial space of the asymmetry skeleton structure realizes lithium metal deposition position and dissolves the accurate regulation and control of position.
Embodiment 6:In mass ratio 9:1 ratio takes graphene powder and Kynoar binder, is added a certain amount of N-Methyl pyrrolidone dispersant carries out dispersion stirring 24 hours, obtains graphene slurry, is scraped using 150 μm of scrapers on copper foil It applies one layer of gained graphene slurry and dries to be made and scrape the copper foil for being coated with graphene.Carbon nanotube powder is taken to be distributed to deionization again In water, dispersion is fully sheared by cutter, carbon nanotube paper can be obtained by being dried after suction filtration, and gained carbon nanotube paper is laid on and is scraped It is coated on the copper foil of graphene to get, porosity difference different to component on thickness direction, conductivity difference, pore structure not The asymmetric skeleton structure of same lithium metal battery cathode.The asymmetry skeleton structure is matched to assembling half-cell with common lithium piece It is tested, electrolyte is lithium hexafluoro phosphate, ethylene carbonate and diethyl carbonate solution.In 1.0mA cm-2Current density and 1.0mAh cm-2Under charge/discharge capacity, which can stablize 50 circle of cycle or more, and coulombic efficiency keeps 91%, passes through scanning electron The interstitial space that the asymmetry skeleton structure can be made full use of when the visible removal lithium embedded in micro- sem observation cathode pole piece section, realizes The accurate regulation and control of lithium metal deposition position and dissolving position.
Embodiment 7:It is small to be dipped in immersion reaction 48 in the ammonium hydroxide of mass fraction 5% for the copper foil for taking 20 μm of a piece of thickness When, one layer of Kocide SD of Surface Creation.The copper foil for taking out Surface Creation Kocide SD is washed and after fully dry water removal, is put into In tube furnace, it is passed through H2With the 1 of Ar:9 mixed gas, and constant temperature carries out reduction reaction in 10 hours at 400 DEG C, finally obtains table Face is by the copper foil of Porous Cu structure composition, and aperture and porosity are increasing to get in thickness from deep to shallow for pore structure On direction with Different Pore Structures, different porosities, different pore size lithium metal battery cathode asymmetric skeleton structure.It should Asymmetric skeleton structure matches assembling half-cell with common lithium piece and is tested, and electrolyte is lithium hexafluoro phosphate, ethylene carbonate With diethyl carbonate solution.In 1.0mA cm-2Current density and 1.0mAh cm-2Under charge/discharge capacity, which, which can stablize, follows More than the circle of ring 80, coulombic efficiency keeps 92%, energy when observing the visible removal lithium embedded in cathode pole piece section by scanning electron microscope The interstitial space for making full use of the asymmetry skeleton structure realizes lithium metal deposition position and dissolves the accurate regulation and control of position.

Claims (5)

1. a kind of asymmetric skeleton structure of lithium metal battery cathode, it is characterised in that:The skeleton structure has in thickness direction Upper inconsistent physicochemical property;Method is prepared the asymmetry skeleton structure one or more of as follows:
A. by physicochemical property it is different multiple material splicing or it is compound after skeleton structure is made;
B. same material is post-processed into the inconsistent rear formation skeleton structure of physicochemical property;
C. direct in-situ prepares the inconsistent material of physicochemical property and forms skeleton structure.
2. a kind of asymmetric skeleton structure of lithium metal battery cathode according to claim 1, it is characterised in that:It is described not Consistent physicochemical property includes that material component is inconsistent, structure is inconsistent, electronic impedance is inconsistent, ionic resistance is inconsistent, electric Solution matter contact angle is inconsistent, molten lithium contact angle is inconsistent, specific surface area is inconsistent, pore size distribution is inconsistent, specific pore volume is inconsistent It is one or more in inconsistent with porosity.
3. a kind of asymmetric skeleton structure of lithium metal battery cathode according to claim 1 or 2, it is characterised in that:Institute Asymmetric skeleton structure is stated to be made of one or both of conductive material and insulating materials.
4. a kind of asymmetric skeleton structure of lithium metal battery cathode according to claim 3, it is characterised in that:It is described to lead Electric material is carbon black, fullerene, graphene, carbon nanotube, template carbon, macropore carbon, hollow carbon balls, activated carbon, carbon fiber, foam It is one or more in carbon, copper, silver, gold, nickel, aluminium, iron and steel.
5. a kind of asymmetric skeleton structure of lithium metal battery cathode according to claim 3, it is characterised in that:It is described exhausted Edge material is polyethylene, polypropylene, polyimides, polymer resin, polyacrylonitrile, polyvinyl chloride, polyethylene oxide, poly- methyl-prop E pioic acid methyl ester, polyaniline, polyether sulfone, Kynoar, Kynoar-hexafluoropropylene copolymer, cellulose acetate, poly- breast It is one or more in acid, polycaprolactone, polytrimethylene carbonate, poly (lactic acid-glycolic acid) and glass fibre.
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CN109713224A (en) * 2018-12-28 2019-05-03 蜂巢能源科技有限公司 Compound lithium an- ode and preparation method, lithium ion battery
CN109994739A (en) * 2019-03-25 2019-07-09 宁德新能源科技有限公司 Cathode pole piece and electrochemical appliance and electronic device comprising it
CN111725480A (en) * 2020-06-29 2020-09-29 珠海冠宇电池股份有限公司 Composite shape memory alloy cathode, preparation method thereof and lithium battery

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CN111725480A (en) * 2020-06-29 2020-09-29 珠海冠宇电池股份有限公司 Composite shape memory alloy cathode, preparation method thereof and lithium battery

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