CN108365200A - A kind of preparation method of compound lithium an- ode - Google Patents
A kind of preparation method of compound lithium an- ode Download PDFInfo
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- CN108365200A CN108365200A CN201810142925.8A CN201810142925A CN108365200A CN 108365200 A CN108365200 A CN 108365200A CN 201810142925 A CN201810142925 A CN 201810142925A CN 108365200 A CN108365200 A CN 108365200A
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
Abstract
The invention discloses a kind of preparation methods of compound lithium an- ode, belong to lithium metal battery technical field.Preparation method is：The surface of framework material is modified first, the framework material with close lithium surface is made, then contacts it with liquid metal lithium, so that liquid metal lithium is fed into the framework material with close lithium surface, compound lithium an- ode is made after cooling.The present invention can make various framework materials (comprising conducting matrix grain material and insulation framework material) obtain compound lithium an- ode material by modified acquisition close lithium surface, and with liquid metal lithium high efficiency composition.When the compound lithium an- ode material obtained is assembled in full battery, lithium dendrite growth can effectively be inhibited, the Volumetric expansion for alleviating cathode, reduces the powder phenomenon-tion of lithium an- ode, greatly improves cyclical stability, safety and the cycle life of lithium metal battery.
Description
Technical field
The present invention relates to a kind of preparation methods of compound lithium an- ode, belong to lithium metal battery technical field.
Background technology
With the high speed development of the industries such as laptop, smart mobile phone, unmanned plane, electric vehicle, it is widely used now
The secondary cells such as lithium ion battery be difficult to meet the needs of today's society is higher and higher to energy-storage system.It finds safer
, the higher electrode material of energy density become current secondary battery research key.Have benefited from lithium metal its high reason
By specific capacity (3860mAh g-1) and minimum oxidation-reduction electrode current potential (- 3.040V vs. standard hydrogen electrodes), lithium metal is negative
Pole becomes most promising next-generation secondary battery cathode material.
But lithium an- ode cannot achieve always large-scale commercial application, the main reason is that filling in lithium metal battery
Electric process, i.e., easily growth forms dendroid or muscoid Li dendrite in the deposition process of lithium metal, this can be to lithium metal battery
Bring problems with：(1) growth of a large amount of dendrite can substantially increase the interfacial area of lithium metal and electrolyte, form exhibiting high surface
It is passivated salt deposit, irreversible capacity loss is brought to lithium metal；(2) dendritic growth is easy puncture diaphragm and causes internal short-circuit of battery,
Reduce battery security；(3) in discharge process dendrite meeting uneven dissolution, and then " the dead lithium " for being detached from negative current collector is formed,
Reduce the active volume of cathode；(4) accumulation of a large amount of " dead lithiums " and surface passivation salt deposit makes lithium anode dusting, and makes entire
Cathode pole piece volume expansion destroys circulating battery stability, battery cycle life is greatly reduced.
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 etc.).These framework materials can very effectively inhibit lithium golden
Belong to the lithium dendrite growth in deposition process, and improve the cycle performance of lithium metal half-cell, but lithium metal can not be applied directly to
In full battery, basic reason is that these framework materials are all free of preset lithium metal, can not be with most of positive electrode
(such as cobalt acid lithium, LiFePO4, sulphur anode, oxygen anode) matching assembles high performance full battery.Therefore, lithium metal is placed in advance
To prepare compound lithium an- ode material in framework material, be realize framework material on lithium metal battery commercial applications must
Through road.Wherein, most easy lithium metal pre-setting method is that lithium metal electroplating deposition is directly entered skeleton material in the electrolyte
In material, however further investigation revealed that containing a large amount of passivation salt deposit impurity by the lithium metal of electroplating deposition so that obtained
Effective lithium content of the composite material obtained is extremely low, cannot be satisfied the high stability of lithium an- ode, the performance requirement of height ratio capacity.
Later, researchers are susceptible to that directly answering containing high-purity lithium metal can be obtained to framework material perfusion fused solution lithium metal
Cathode is closed, and then effectively solves the problems, such as lithium content, but finds that most of framework material all can not be with liquid in practical operation
Lithium metal is affine, can not lithium metal directly be sucked skeleton.Therefore, liquid metal lithium can be fed into any bone by design one kind
The compound lithium metal battery cathode preparation method of frame material is the active demand of lithium metal battery commercial applications.
Invention content
The object of the present invention is to provide a kind of preparation method of compound lithium an- ode, this method can make common various
Framework material (including conducting matrix grain material and insulation framework material) realizes high efficiency composition by modified with liquid metal lithium, obtains
Obtain the compound lithium an- ode material containing preset high-purity lithium.
Technical scheme is as follows：
A kind of preparation method of compound lithium an- ode, it is characterised in that this method comprises the following steps：
1) surface of the framework material of lithium an- ode is modified, the framework material with close lithium surface is made.
2) solid-state lithium is heated to 190 DEG C~1330 DEG C, lithium metal is made to be mixed with the framework material with close lithium surface, it is cold
But compound lithium an- ode is made afterwards so that mass fraction of the lithium metal in composite negative pole is 40%~95%.
Framework material of the present invention is one or more in framework material, insulation framework material.
Preferably, the framework material is one in graphene, carbon nanotube, carbon fiber, copper, nickel, aluminium, iron and stainless steel
Kind is a variety of.
Preferably, the insulation framework material is polyethylene, polypropylene, polyimides, polymer resin, polyacrylonitrile, gathers
Vinyl chloride, polyethylene oxide, polymethyl methacrylate, polyaniline, polyether sulfone, Kynoar, Kynoar-hexafluoro third
In alkene copolymer, cellulose acetate, polylactic acid, polycaprolactone, polytrimethylene carbonate, poly (lactic acid-glycolic acid) and glass fibre
It is one or more.
Modification of the present invention includes one or more in physical modification, chemical modification, coating modification.The physics changes
Property include mechanical processing, laser processing, electron beam process, ion beam processing it is one or more.The chemical modification includes table
Face oxidation, the phosphorous functional group of addition, adds the one or more of siliceous functional group at surfaces nitrided, surface fluorination, surface sulfide.
The coating modification includes will be one or more in the metal material of close lithium, inorganic matter containing lithium, inorganic matter containing magnesium and oxide
Deposition material by one kind in spraying, vapor deposition, sputtering, plating, chemistry displacement, liquid phase chemical deposition and chemical vapor deposition or
The modification that kinds of processes carries out.
The method that liquid metal lithium of the present invention is mixed with the framework material with close lithium surface includes being in direct contact, surpassing
It is one or more in sound, oscillation, shearing, stirring and fluidizing method.
The present invention compared with prior art, has the following advantages that and high-lighting effect：By this technology, various skeletons can be made
Material (comprising all kinds of conducting matrix grain materials and insulation framework material), and can be with liquid metal by modified acquisitions parent's lithium surface
Lithium realizes high efficiency composition, obtains compound lithium metal battery negative material.The compound lithium metal battery negative material obtained contains
Controllable effective lithium metal content (lithium metal mass fraction can be effectively controlled 40%-95%).The compound lithium metal obtained
It when cell negative electrode material is assembled in lithium metal full battery, can effectively inhibit lithium dendrite growth, reduce the dusting of lithium an- ode
Phenomenon greatly improves the cyclical stability of lithium metal battery, safety, cycle life.
Specific implementation mode
A kind of preparation method of compound lithium an- ode provided by the invention, specifically comprises the following steps：
1) the framework material surface of lithium an- ode is modified, the framework material with close lithium surface is made；
2) solid-state lithium is heated to 190 DEG C~1330 DEG C, so that lithium metal is mixed with the framework material with close lithium surface, mixes
The method of conjunction includes being in direct contact, being in ultrasound, oscillation, shearing, stirring or fluidizing method one or more；Postcooling be made
Compound lithium an- ode so that mass fraction of the lithium metal in composite negative pole is 40%~95%.
The framework material is conducting matrix grain material or insulation framework material, and the conducting matrix grain material is graphene, carbon
It is one or more in nanotube, carbon fiber, copper, nickel, aluminium, iron and stainless steel；The insulation framework material is polyethylene, poly- third
Alkene, polymer resin, polyacrylonitrile, polyvinyl chloride, polyethylene oxide, polymethyl methacrylate, polyaniline, gathers polyimides
Ether sulfone, Kynoar, Kynoar-hexafluoropropylene copolymer, cellulose acetate, polylactic acid, polycaprolactone, poly- three methylene
It is one or more in base carbonic ester, poly (lactic acid-glycolic acid) and glass fibre.
It is of the present invention that framework material surface is modified including in the modification of physical modification, chemical modification and coating
It is one or more.The physical modification include mechanical processing, laser processing, electron beam process and one kind in ion beam processing or
It is a variety of.The chemical modification includes surface oxidation, surfaces nitrided, surface fluorination, surface sulfide, the phosphorous functional group of addition and addition
Siliceous functional group it is one or more.The coating be modified include by the metal material of close lithium (including sodium, magnesium, titanium, zirconium, chromium,
Molybdenum, iron, nickel, copper, silver, gold, zinc, aluminium), inorganic matter containing lithium (including lithium fluoride, lithium chloride, lithium nitride, lithia), containing magnesium it is inorganic
Object (magnesium fluoride, magnesium nitride, magnesia), oxide (including titanium dioxide, zirconium dioxide, copper oxide, silver oxide, zinc oxide, oxygen
Change aluminium, silica) in one or more deposition materials pass through spraying, vapor deposition, sputtering, plating, chemistry displacement, liquid phase chemical
One or more techniques in deposition, chemical vapor deposition are modified.
The present invention is described further with reference to specific embodiment, so that those skilled in the art are further
Understand the present invention.
Embodiment 1：It takes graphene powder to be put into tube furnace, is passed through H2With NH32:1 mixed gas, the constant temperature 1 at 600 DEG C
Hour carries out N doping reaction, and the nitrogen-doped graphene that N doping amount is atomic fraction 2% is made, which is compressed to
The self-supporting pole piece of 500 μ m-thicks.The pole piece is put into 400 DEG C of molten metal lithiums in argon gas atmosphere, molten lithium can be filled voluntarily
Nitrogen-doped graphene skeleton is injected, the compound lithium an- ode material that average lithium metal mass fraction is 82% is obtained after taking out cooling
Material.The compound lithium an- ode material is matched assembling full battery with iron phosphate lithium positive pole to test, electrolyte is hexafluoro phosphorus
Sour lithium, ethylene carbonate and diethyl carbonate solution.Under 1C multiplying powers, which can stablize 500 circle of cycle or more, and capacity is kept
Rate is up to 74%.The compound lithium an- ode material after charge and discharge is observed by scanning electron microscope, finds no dendrite life
It is long, also without powder phenomenon-tion.
Embodiment 2：It is put into the magnesium oxide template for being loaded with Fe catalyst in tube furnace, is passed through H2、CH4With NH32:7:1
Mixed gas, constant temperature 5 hours at 900 DEG C, to prepare situ Nitrogen Doping carbon nanotube.Extra mass score is added in gained powder
The stirring of 10% dilute hydrochloric acid dipping is to dissolve removal Fe catalyst and magnesium oxide template, and insoluble matter is after filtration washing is dried up to nitrogen
Doped carbon nanometer pipe powder.The powder is melted with lithium metal block at 190 DEG C in argon gas atmosphere, and is sufficiently stirred, makes to melt
Melt lithium to be sufficiently mixed with nitrogen doped carbon nanotube powder, obtains pouring into the nitrogen doped carbon nanotube powder of lithium metal after cooling.By gained
Pressed powder, is made the compound lithium an- ode material of 500 μm of thickness, and lithium metal mass fraction is 40%.By the complex lithium
Metal negative electrode material matches assembling full battery with iron phosphate lithium positive pole and is tested, and electrolyte is lithium hexafluoro phosphate, ethylene carbonate
Ester and diethyl carbonate solution.Under 1C multiplying powers, which can stablize 500 circle of cycle or more, and capacity retention ratio is up to 68%.It is logical
The compound lithium an- ode material after electron microscope observation charge and discharge is over-scanned, no dendritic growth is found, also without dusting
Phenomenon.
Embodiment 3：Using gold target as target source, 200 μ m-thicks carbon fiber paper surface ion sputtering a layer thickness about
The gold plating of 50nm.The gold-plated carbon fiber paper is put into 600 DEG C of molten metal lithiums in argon gas atmosphere, molten lithium can be filled voluntarily
It injects in gold-plated carbon fiber paper skeleton, the compound lithium an- ode material that lithium metal mass fraction is 90% is obtained after taking out cooling
Material.The compound lithium an- ode material is matched assembling full battery with iron phosphate lithium positive pole to test, electrolyte is hexafluoro phosphorus
Sour lithium, ethylene carbonate and diethyl carbonate solution.Under 1C multiplying powers, which can stablize 700 circle of cycle or more, and capacity is kept
Rate is up to 83%.The compound lithium an- ode material after charge and discharge is observed by scanning electron microscope, finds no dendrite life
It is long, also without powder phenomenon-tion.
Embodiment 4：The copper mesh of 500 μm of thickness, 200 mesh numbers is immersed into the silver nitrate solution that mass fraction is 0.1%, reaction
It is removed and placed in deionized water after 10 seconds and fully washs, take out drying, obtain the silver-plated copper mesh prepared by chemical displacement method.
It is put it into argon gas atmosphere in 1330 DEG C of molten metal lithiums, molten lithium can voluntarily be fed into silver-plated copper network framework, take out cold
But the compound lithium an- ode material that lithium metal mass fraction is 95% is obtained afterwards.By the compound lithium an- ode material and phosphoric acid
Iron lithium anode matching assembling full battery is tested, and electrolyte is lithium hexafluoro phosphate, ethylene carbonate and diethyl carbonate solution.
Under 1C multiplying powers, which can stablize 400 circle of cycle or more, and capacity retention ratio is up to 82%.It is seen by scanning electron microscope
The compound lithium an- ode material after charge and discharge is examined, no dendritic growth is found, also without powder phenomenon-tion.
Embodiment 5：The foam copper that thickness is 1mm is put into tube furnace, O is passed through2With N21:9 mixed gas, 300
Constant temperature carries out surface oxidation reaction in 1 hour at DEG C, obtains the oxidation foam copper skeleton of surface covering copper oxide.In argon gas atmosphere
It puts it into 800 DEG C of molten metal lithiums, molten lithium can voluntarily be fed into oxidation foam copper skeleton, and lithium gold is obtained after taking out cooling
Belong to the compound lithium an- ode material that mass fraction is 56%.The compound lithium an- ode material is matched with iron phosphate lithium positive pole
Assembling full battery is tested, and electrolyte is lithium hexafluoro phosphate, ethylene carbonate and diethyl carbonate solution.Under 1C multiplying powers,
The battery can stablize 500 circle of cycle or more, and capacity retention ratio is up to 70%.After charge and discharge being observed by scanning electron microscope
Compound lithium an- ode material, finds no dendritic growth, also without powder phenomenon-tion.
Embodiment 6：Using magnesia as target, by magnetron sputtering in the foam nickel surface sputtering one that thickness is 1mm
The magnesium oxide coating of layer thickness about 80nm.It is put it into argon gas atmosphere in 500 DEG C of molten metal lithiums, molten lithium can be filled voluntarily
Injection is coated with the foam nickel skeleton of magnesia, and the compound lithium an- ode that lithium metal mass fraction is 75% is obtained after taking out cooling
Material.The compound lithium an- ode material is matched assembling full battery with iron phosphate lithium positive pole to test, electrolyte is hexafluoro
Lithium phosphate, ethylene carbonate and diethyl carbonate solution.Under 1C multiplying powers, which can stablize 450 circle of cycle or more, and capacity is protected
Holdup is up to 71%.The compound lithium an- ode material after charge and discharge is observed by scanning electron microscope, finds no dendrite
Growth, also without powder phenomenon-tion.
Embodiment 7：Using zinc target as target, a layer thickness is sputtered about in the all-glass paper surface ion of 1mm thickness
The spelter coating of 100nm.It is put it into argon gas atmosphere in 300 DEG C of molten metal lithiums, molten lithium can voluntarily be fed into zinc-plated
Glass fibre skeleton obtains the compound lithium an- ode material that lithium metal mass fraction is 79% after taking out cooling.This is compound
Lithium an- ode material matches assembling lithium sulphur full battery with sulphur anode and is tested, and electrolyte is bis trifluoromethyl sulfimide
Lithium, 1,3- dioxolanes, ethylene glycol dimethyl ether solution.Under 0.5C multiplying powers, which can stablize 200 circle of cycle or more, capacity
Conservation rate is up to 83%.The compound lithium an- ode material after charge and discharge is observed by scanning electron microscope, discovery does not have branch
Crystals growth, also without powder phenomenon-tion.
Embodiment 8：The stainless steel foam that thickness is 1mm is connected cathode to be put into electroplating pool, anode is silver plate, electroplate liquid
The silver nitrate aqueous solution for being 2% for mass fraction is passed through 100mA cm-2Electroplating current, be electroplated 1 minute, obtain silver-plated bubble
Foam stainless steel material.It is put it into argon gas atmosphere in 900 DEG C of molten metal lithiums, molten lithium can voluntarily be fed into silver-plated foam
Stainless steel insert obtains the compound lithium an- ode material that lithium metal mass fraction is 85% after taking out cooling.By the complex lithium
Metal negative electrode material matched with sulphur anode assembling lithium sulphur full battery tested, electrolyte be bis trifluoromethyl sulfimide lithium,
1,3- dioxolanes, ethylene glycol dimethyl ether solution.Under 0.5C multiplying powers, which can stablize 300 circle of cycle or more, and capacity is kept
Rate is up to 81%.The compound lithium an- ode material after charge and discharge is observed by scanning electron microscope, finds no dendrite life
It is long, also without powder phenomenon-tion.
Claims (9)
1. a kind of preparation method of compound lithium an- ode, it is characterised in that this method comprises the following steps：
1) the framework material surface of lithium an- ode is modified, the framework material with close lithium surface is made；
2) solid-state lithium is heated to 190 DEG C~1330 DEG C, so that lithium metal is mixed with the framework material with close lithium surface, after cooling
Compound lithium an- ode is made so that mass fraction of the lithium metal in composite negative pole is 40%~95%.
2. a kind of preparation method of compound lithium an- ode according to claim 1, it is characterised in that：The framework material
For conducting matrix grain material or insulation framework material.
3. a kind of preparation method of compound lithium an- ode according to claim 2, it is characterised in that：The conducting matrix grain
Material is one or more in graphene, carbon nanotube, carbon fiber, copper, nickel, aluminium, iron and stainless steel.
4. a kind of preparation method of compound lithium an- ode according to claim 2, it is characterised in that：The insulation framework
Material is polyethylene, polypropylene, polyimides, polymer resin, polyacrylonitrile, polyvinyl chloride, polyethylene oxide, polymethyl
Sour methyl esters, polyaniline, polyether sulfone, Kynoar, Kynoar-hexafluoropropylene copolymer, cellulose acetate, polylactic acid,
It is one or more in polycaprolactone, polytrimethylene carbonate, poly (lactic acid-glycolic acid) and glass fibre.
5. a kind of preparation method of compound lithium an- ode according to claim 1-4 any claims, feature exist
In：The framework material surface is modified one or more in being modified including physical modification, chemical modification and coating.
6. a kind of preparation method of compound lithium an- ode according to claim 5, it is characterised in that：The physical modification
Including one or more in mechanical processing, laser processing, electron beam process and ion beam processing.
7. a kind of preparation method of compound lithium an- ode according to claim 5, it is characterised in that：The chemical modification
Including surface oxidation, surfaces nitrided, surface fluorination, surface sulfide, the phosphorous functional group of addition and the one kind for adding siliceous functional group
Or it is a variety of.
8. a kind of preparation method of compound lithium an- ode according to claim 5, it is characterised in that：The coating is modified
Include that one or more deposition materials in close lithium metal material, inorganic matter containing lithium, inorganic matter containing magnesium and oxide are passed through into spray
It applies, one or more techniques in vapor deposition, sputtering, plating, chemistry displacement, liquid phase chemical deposition and chemical vapor deposition are changed
Property.
9. a kind of preparation method of compound lithium an- ode according to claim 1, it is characterised in that：Liquid metal lithium with
The method of framework material mixing with close lithium surface includes being in direct contact, in ultrasound, oscillation, shearing, stirring or fluidizing method
It is one or more.
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