CN106384838A - Atomic layer deposition modified lithium-ion battery and preparation method thereof - Google Patents
Atomic layer deposition modified lithium-ion battery and preparation method thereof Download PDFInfo
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- CN106384838A CN106384838A CN201610957447.7A CN201610957447A CN106384838A CN 106384838 A CN106384838 A CN 106384838A CN 201610957447 A CN201610957447 A CN 201610957447A CN 106384838 A CN106384838 A CN 106384838A
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- ion battery
- ald
- decorative layer
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- negative 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0421—Methods of deposition of the material involving vapour deposition
- H01M4/0428—Chemical vapour deposition
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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
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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 an atomic layer deposition (ALD) modified lithium-ion battery and a preparation method thereof. According to the atomic layer deposition modified lithium-ion battery disclosed by the invention, a modification layer is formed on at least one surface of a positive electrode active material and a negative electrode active material; each modification layer is formed through adopting an atomic layer deposition process; or a modification layer is formed at least one surface of a positive electrode pole piece and a negative electrode pole piece, and each modification layer is formed through adopting the atomic layer deposition process.
Description
Technical field
The present invention relates to lithium-ions battery；The lithium ion battery modified particularly to a kind of ald and its preparation
Method.
Background technology
Lithium-ions battery since 1991 be commercialized since, with its high-energy-density, high working voltage, low self-discharge efficiency
And the advantages of memory-less effect, attracted extensive concern sight.Lithium-ions battery has been widely used for traffic, leads at present
The multiple fields such as letter, the energy.But when applying to space field, the cyclical stability of existing lithium ion battery and heat-resisting quantity
The requirement of Space-Work environment can not be met.
Content of the invention
During the problem that the present invention solves, the cyclical stability of existing lithium ion battery and heat-resisting quantity are not good, for solution
Certainly described problem, the present invention provides a kind of lithium ion battery of ald modification and preparation method thereof.
The positive and negative electrode active material of the lithium ion battery that the ald that the present invention provides is modified at least selects a table
Face is formed with decorative layer, and described decorative layer is formed using atom layer deposition process；Or positive and negative electrode pole piece at least selects a surface shape
Become to have decorative layer, described decorative layer is formed using atom layer deposition process.
Further, the material of described decorative layer includes：Al2O3, SiO2, RuO2, CeO2, MgO, SrTiO3, TiO2, ZrO2,
AlF3, CaF2, MgF2, SrF2, ZnF2One or more of.
Further, the thickness of the decorative layer being formed using atom layer deposition process is 10-350 deposition cycle.
The present invention also provides the preparation method of the described lithium ion battery of ald modification, including：Step one, adopt
With ald (ALD) technique, at least select one surface deposition decorative layer in anode and cathode active materials；Step 2, adopt institute
State anode and cathode active materials and prepare positive and negative electrode pole piece respectively.
Further, the material of described decorative layer includes：Al2O3, SiO2, RuO2, CeO2, MgO, SrTiO3, TiO2, ZrO2,
AlF3, CaF2, MgF2, SrF2, ZnF2One or more of.
The present invention also provides the preparation method of the described lithium ion battery of ald modification, including：Step one, adopt
With atom layer deposition process, at least select the surface deposition decorative layer of an electrode in positive and negative electrode；Step 2, adopt described positive and negative electrode
Prepare lithium ion battery.
Further, the material of described decorative layer includes：Al2O3, SiO2, RuO2, CeO2, MgO, SrTiO3, TiO2, ZrO2,
AlF3, CaF2, MgF2, SrF2, ZnF2One or more of
Further, depositing operation includes：Cavity internal gas pressure is 1-2 Pa, -230 DEG C of temperature 50 C, and the burst length of precursor sets
It is set to 5 ~ 30ms, the washing time of precursor is set to 5 ~ 30 s, carrier gas flux 10-30 SCCM.
Beneficial effects of the present invention include：
（1）High stability electrode/electrolyte interface：Based on ald modification technique, construct and stabilize electrode/electrolyte
Boundary layer, improves high temperature and the cyclical stability of battery.
（2）Atomic layer deposition thin film thickness controllable precise：Determined by the cycle-index depositing, you can be reacted by control
The thickness of periodicity precise control film, thus reach the film of atomic layer level thickness precision；Ald have good film-forming property,
The advantages of growth temperature is low, good crystallinity, chemical composition are controlled, thickness is easily-controllable and receive much concern, can be used for electrode material
Nanosizing is modified.
Brief description
Fig. 1 is the lithium ion battery rate discharge curves that ald provided in an embodiment of the present invention is modified；
Fig. 2 is the electrodes of lithium-ion batteries heat endurance that ald provided in an embodiment of the present invention is modified；
Fig. 3 is the high-temperature lithium ion battery cycle performance that ald provided in an embodiment of the present invention is modified.
Specific embodiment
From background technology, the cyclical stability of existing lithium ion battery and hot properties are not good；Inventor is directed to
Described problem is studied it is believed that being because the interface performance of positive and negative plate and electrolyte produces to the performance of lithium ion battery
Impact, stable nanocrystalline surface layer is an approach solving effect of the interface.
ALD growth course is the surface by selectively alternately different presomas being exposed to substrate, in surface chemistry
Adsorb and react and form deposition film.Compared with traditional chemical vapour deposition technique CVD, ALD technique requires strictly to hold
Row ALT pulse presoma, to avoid the process of gas phase reaction.Due to having, simple, repeatable, conformality is good and film thickness
In the advantage such as nanoscale is adjustable.
ALD technology is applied to lithium ion battery technology by inventor, provides a kind of ald to modify in the present invention
Lithium ion battery and preparation method thereof.
Hereinafter, the present invention is further elaborated in conjunction with the accompanying drawings and embodiments.
Lithium ion battery provided in an embodiment of the present invention includes positive and negative electrode pole piece, barrier film, electrolyte, external packing.Described
Selecting a surface in positive and negative electrode pole piece adopts ALD to form decorative layer；The material of described decorative layer selects：Al2O3, SiO2, RuO2,
CeO2, MgO, SrTiO3, TiO2, ZrO2, AlF3, CaF2, MgF2, SrF2, ZnF2One or more of.Another reality of the present invention
Apply in example, first any one in anode and cathode active materials, or two kinds of surface adopts ALD technique to form decorative layer, then
One of anode pole piece and cathode pole piece or two kinds are prepared using the active material comprising decorative layer；The material of described decorative layer
Material selects：Al2O3, SiO2, RuO2, CeO2, MgO, SrTiO3, TiO2, ZrO2, AlF3, CaF2, MgF2, SrF2, ZnF2In one
Plant or multiple.Described ald decorative layer thickness is 10-350 deposition cycle.
Described positive active material selects Ni-based ternary and its material modified, and nickel cobalt binary positive pole is material modified, high pressure
Cobalt acid lithium, rich lithium material and its material modified in any one or more；This negative electrode active material selects carbonaceous mesophase spherules,
High power capacity graphite, one or more of silica-base material.
First embodiment of the invention provides the preparation method of the lithium ion battery of described ald modification, comprises
Step one, adopt ald (ALD) technique, anode and cathode active materials at least select one surface deposition decorative layer；
Step 2, prepare positive and negative electrode respectively using described anode and cathode active materials.The step preparing positive pole includes：By N- methylpyrrole
Alkanone（NMP）And polyvinylidene fluoride（PVDF）Mix and blend certain time, add positive conductive agent, be eventually adding atomic layer
The positive electrode active materials modified or unmodified positive electrode active materials, above-mentioned slurry are coated on aluminium foil surface, dry
To positive pole；Prepare negative pole to include：By sodium carboxymethylcellulose（CMC）Carry out mix and blend certain time with distilled water, add negative
Pole conductive agent, is subsequently adding the negative electrode active material of atomic layer modification or unmodified negative electrode active material, is eventually adding butylbenzene
Rubber（SBR）, the slurry of gained is coated to copper foil surface, dries and can get negative pole.
Step 3：The positive pole of gained and negative pole are rolled into certain thickness, are punched into a certain size pole piece, then will
Anode pole piece and cathode pole piece replace accumulation, and centre barrier film separates, and finally all of positive pole ear is welded together extraction
Positive pole ear, negative lug welds together extraction negative lug.Now obtain battery battery core.
Step 4：Above-mentioned battery core is packed with aluminum plastic film, and is carried out baking and removed moisture.
Step 5：Inject certain electrolyte in above-mentioned battery core, and seal and shelve certain time.
Step 6：Discharge and recharge is carried out to battery, and carries out vacuumizing away gas.
Step 7：Battery is charged with small current, is discharged with high current.
Second embodiment of the invention also provides the preparation method of the described lithium ion battery of ald modification, bag
Include：Step one, adopt atom layer deposition process, at least select the surface deposition decorative layer of an electrode in positive and negative electrode；Step 2, adopt
Prepare lithium ion battery with described positive and negative electrode.
Further, depositing operation includes：Cavity internal gas pressure is 1-2 Pa, -500 DEG C of temperature 50 C, such as 100 DEG C, 180
℃；The burst length of precursor is set to 5 ~ 30ms, and the washing time of precursor is set to 5 ~ 30 s, such as adopts TMA and H2O
As presoma, the burst length of presoma is disposed as 10ms, and the washing time of TMA is set to 10 s, H2The washing time of O
It is set to 15 s, carrier gas flux 10-30 SCCM.
Embodiment 1
The viscosity of 60 grams of 1-METHYLPYRROLIDONEs and 3 grams of polyvinylidene fluoride mix and blends mixed liquors up within 10 minutes is become
Change be less than 3%, add 1 gram particle footpath be less than 5 microns microspheroidal superconduction carbon black, 1g pipe range be less than 100 microns CNT and
1 gram of flakey electrically conductive graphite stirs within 10 minutes mixture viscosity change and is less than 3%, is eventually adding 94 grams through atomic layer
The LiNi of 25 circulations of surface modification0.80Co0.15Al0.05O2Material, stirring mixture viscosity change up within 10 minutes is little
In 5%, then above-mentioned solidliquid mixture is coated on aluminium foil, 100 DEG C vacuum drying 24 hours after obtain positive electrode.By 100 grams
The viscosity B coefficent of distilled water and 1.5 grams of sodium carboxymethylcellulose mix and blends mixed liquors up within 10 minutes is less than 3%, then
The microspheroidal superconduction carbon black that 3 gram particle footpaths are less than 5 microns and 1g flakey electrically conductive graphite is added to stir the mixture within 10 minutes
Viscosity B coefficent is less than 3%, adds 95 grams of graphite cathode materials having modified 25 circulations through atomic level surface and stirs up to 10
Within minute, mixture viscosity change is less than 3%, is subsequently adding 2.5g butadiene-styrene rubber（SBR）Stirring mixture up in 10 minutes
Viscosity B coefficent is less than 3%, finally above-mentioned solidliquid mixture is coated on Copper Foil, 100 DEG C of vacuum drying post-drying preparation in 24 hours
Negative electrode.By the positive and negative electrode of above-mentioned making after being rolled into certain thickness, it is cut into the small pieces of definite shape, if will
Dry positive and negative electrode small pieces are piled up successively with both positive and negative polarity over-over mode, are insulated with barrier film between positive and negative electrode, and respectively on aluminium foil
Welding aluminium strip, Copper Foil welds nickel strap, and finally makes positive and negative electrode avoid electronic conduction using the fixing positive and negative electrode of adhesive tape, does
Become battery core.Then, battery core is put into external packing, remove moisture in a vacuum.Toward dewatered equipped with the external packing of battery core
Add 25g electrolyte, seal and stand, make electrolyte fully infiltrate the solid particle on aluminium foil and Copper Foil.Carried out with small current
Discharge and recharge is melted into.And the row's of closing gas passage, obtain the flexible package ion accumulator that capacity is 5Ah.Battery is with 1A constant-current charge
To 4.2V, turn constant voltage 4.2V and charge to electric current less than 0.1A, after standing 10min, respectively with 1A, 5A, 10A, 15A and 25A constant current
It is discharged to 2.75V, its rate discharge curves is as shown in Figure 1.
Embodiment 2
The viscosity of 60 grams of 1-METHYLPYRROLIDONEs and 3 grams of polyvinylidene fluoride mix and blends mixed liquors up within 10 minutes is become
Change be less than 3%, add 1 gram particle footpath be less than 5 microns microspheroidal superconduction carbon black, 1g pipe range be less than 100 microns CNT and
1 gram of flakey electrically conductive graphite stirs within 10 minutes mixture viscosity change and is less than 3%, is just being eventually adding 94 grams of nickel cobalt binary
Pole material, stirring mixture viscosity change up within 10 minutes is less than 5%, then above-mentioned solidliquid mixture is coated on aluminium foil
On, 100 DEG C vacuum drying 24 hours after obtain positive electrode.By 100 grams of distilled water and 1.5 grams of sodium carboxymethylcellulose mix and blends
Until the viscosity B coefficent of mixed liquor is less than 3% within 10 minutes, it is subsequently adding the microspheroidal superconduction carbon black that 3 gram particle footpaths are less than 5 microns
Stir within 10 minutes mixture viscosity change with 1g flakey electrically conductive graphite and be less than 3%, add 95 grams of graphite cathode stirrings
Until mixture viscosity change is less than 3% within 10 minutes, it is subsequently adding 2.5g butadiene-styrene rubber（SBR）Stirring is up in 10 minutes
Mixture viscosity change be less than 3%, finally above-mentioned solidliquid mixture is coated on Copper Foil, 100 DEG C vacuum drying 24 hours after dry
Drying standby negative electrode.By the positive and negative electrode of above-mentioned making after being rolled into certain thickness, it is cut into the little of definite shape
Piece, then positive pole small pieces are carried out 50 and 300 cycle atomic layer deposition, by the positive pole having deposited small pieces and negative pole small pieces with just
Negative pole over-over mode is piled up successively, is insulated with barrier film, and welds aluminium strip on aluminium foil respectively, Copper Foil welds between positive and negative electrode
Connect nickel strap, and finally make positive and negative electrode avoid electronic conduction using the fixing positive and negative electrode of adhesive tape, make battery core.Then, by electricity
External packing put into by core, removes moisture in a vacuum.Add 25g electrolyte toward dewatered equipped with the external packing of battery core, seal
Mouth simultaneously stands, and makes electrolyte fully infiltrate the solid particle on aluminium foil and Copper Foil.Discharge and recharge chemical conversion is carried out with small current.And close
Row's gas passage, obtains the flexible package ion accumulator that capacity is 5Ah.Battery turns constant voltage 4.2V with 1A constant-current charge to 4.2V
Charge to electric current and be less than 0.1A, after standing 10min, respectively with 1A, 5A, 10A, 15A and 25A constant-current discharge to 2.75V.Atomic layer
Deposit the electrodes of lithium-ion batteries heat endurance before and after modifying as shown in Fig. 2 pole piece heat endurance shows after ald is modified
Write and provide, its rate of heat release and heat reduce.
Embodiment 3
The viscosity of 60 grams of 1-METHYLPYRROLIDONEs and 3 grams of polyvinylidene fluoride mix and blends mixed liquors up within 10 minutes is become
Change be less than 3%, add 1 gram particle footpath be less than 5 microns microspheroidal superconduction carbon black, 1g pipe range be less than 100 microns CNT and
1 gram of flakey electrically conductive graphite stirs within 10 minutes mixture viscosity change and is less than 3%, is eventually adding 94 grams of high pressure cobalt acid lithiums,
Stirring mixture viscosity change up within 10 minutes is less than 5%, then above-mentioned solidliquid mixture is coated on aluminium foil, 100 DEG C
Vacuum drying obtained positive electrode after 24 hours.By 100 grams of distilled water and 1.5 grams of sodium carboxymethylcellulose mix and blends up to 10 points
Within clock, the viscosity B coefficent of mixed liquor is less than 3%, is subsequently adding microspheroidal superconduction carbon black and the 1g scale that 3 gram particle footpaths are less than 5 microns
Shape electrically conductive graphite stirs within 10 minutes mixture viscosity change and is less than 3%, adds 95 grams of graphite cathode stirrings up to 10 points
Within clock, mixture viscosity change is less than 3%, is subsequently adding 2.5g butadiene-styrene rubber（SBR）Stirring mixture up in 10 minutes glues
Degree change is less than 3%, finally above-mentioned solidliquid mixture is coated on Copper Foil, and 100 DEG C of vacuum drying post-drying preparation in 24 hours is negative
Electrode.By the positive and negative electrode of above-mentioned making after being rolled into certain thickness, it is cut into the small pieces of definite shape, then will bear
Minimum carries out 50 cycle atomic layer deposition, by the negative pole having deposited small pieces and positive pole small pieces with both positive and negative polarity over-over mode successively
Pile up, insulated with barrier film between positive and negative electrode, and weld aluminium strip on aluminium foil respectively, Copper Foil welds nickel strap, and finally uses
The fixing positive and negative electrode of adhesive tape makes positive and negative electrode avoid electronic conduction, makes battery core.Then, battery core is put into external packing, true
Aerial removing moisture.Add 25g electrolyte toward dewatered equipped with the external packing of battery core, seal and stand, make electrolyte
Solid particle fully on infiltration aluminium foil and Copper Foil.Discharge and recharge chemical conversion is carried out with small current.And the row's of closing gas passage, obtain and hold
Measure the flexible package ion accumulator for 5Ah.Battery to 4.2V, is turned constant voltage 4.2V and charges to electric current and be less than with 1A constant-current charge
0.1A, after standing 10min, respectively with 1A, 5A, 10A, 15A and 25A constant-current discharge to 2.75V.Before and after ald is modified
High-temperature lithium ion battery cycle performance as shown in figure 3, ald modify before under the conditions of 55 DEG C, 1C/1C discharge and recharge, 200
After secondary circulation, capability retention is reduced to 80%, and after ald is modified, under the same terms, its cycle-index improves to 400
Secondary, performance boost 100%.
To sum up, using scheme provided in an embodiment of the present invention, the cycle performance of lithium ion battery and heat resistance are carried
High.
Although the present invention is open as above with preferred embodiment, it is not for limiting the present invention, any this area
Without departing from the spirit and scope of the present invention, the methods and techniques content that may be by the disclosure above is to this for technical staff
Bright technical scheme makes possible variation and modification, and therefore, every content without departing from technical solution of the present invention, according to the present invention
Technical spirit any simple modification, equivalent variations and modification that above example is made, belong to technical solution of the present invention
Protection domain.
Claims (7)
1. the lithium ion battery that a kind of ald is modified is it is characterised in that positive and negative electrode active material at least selects a table
Face is formed with decorative layer, and described decorative layer is formed using atom layer deposition process；Or positive and negative electrode pole piece at least selects a surface shape
Become to have decorative layer, described decorative layer is formed using atom layer deposition process.
2. the lithium ion battery modified according to the ald described in claim 1 is it is characterised in that the material of described decorative layer
Material includes：Al2O3, SiO2, RuO2, CeO2, MgO, SrTiO3, TiO2, ZrO2, AlF3, CaF2, MgF2, SrF2, ZnF2In one
Plant or multiple.
3. the lithium ion battery that the ald described in foundation claim 1 is modified is it is characterised in that adopt ald
The thickness of the decorative layer that technique is formed is 10-350 deposition cycle.
4. the preparation method of the lithium ion battery that the ald that in claims 1 to 3, any one is provided is modified, it is special
Levy and be, including：Step one, adopt atom layer deposition process, the surface deposition at least selecting in anode and cathode active materials is modified
Layer；Step 2, prepare positive and negative electrode pole piece respectively using described anode and cathode active materials.
5. according to the preparation method described in claim 4 it is characterised in that the material of described decorative layer includes：Al2O3, SiO2,
RuO2, CeO2, MgO, SrTiO3, TiO2, ZrO2, AlF3, CaF2, MgF2, SrF2, ZnF2One or more of.
6. the preparation method of the lithium ion battery that the ald that in Claims 1-4, any one is provided is modified, it is special
Levy and be, including：Step one, adopt atom layer deposition process, at least select the surface deposition decorative layer of an electrode in positive and negative electrode；
Step 2, lithium ion battery is prepared using described positive and negative electrode.
7. according to the preparation method described in claim 6 it is characterised in that the material of described decorative layer includes：Al2O3, SiO2,
RuO2, CeO2, MgO, SrTiO3, TiO2, ZrO2, AlF3, CaF2, MgF2, SrF2, ZnF2One or more of
According to the preparation method described in claim 6 it is characterised in that depositing operation includes：Cavity internal gas pressure is 1-2 Pa, temperature
50 DEG C -500 DEG C of degree, the burst length of precursor is set to 5 ~ 30ms, and the washing time of precursor is set to 5 ~ 30 s, carrier gas stream
Amount 10-30 SCCM.
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