CN108110324A - A kind of preparation method of solid lithium ion battery - Google Patents
A kind of preparation method of solid lithium ion battery Download PDFInfo
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- CN108110324A CN108110324A CN201711147849.1A CN201711147849A CN108110324A CN 108110324 A CN108110324 A CN 108110324A CN 201711147849 A CN201711147849 A CN 201711147849A CN 108110324 A CN108110324 A CN 108110324A
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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
- H01M10/058—Construction or manufacture
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of electrolyte
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The embodiment of the present invention provides a kind of preparation method of solid lithium ion battery, is related to battery preparation technology field.This method includes：Solid electrolyte is placed in solvent and is disperseed, obtains solid electrolyte solution, wherein, the mass ratio of solid electrolyte and solvent is 1:5~50；Anode of the ternary material as solid lithium ion battery is chosen, lithium metal is as cathode；Film forming agent is added in solid electrolyte solution, and the surface coated on anode and cathode, it is dry, and the anode for being coated with solid electrolyte is sintered under conditions of 800~1000 DEG C, 2~10h is kept the temperature, is cooled down, wherein, film forming agent is polyvinylidene fluoride, polytetrafluoroethylene (PTFE) or polyvinyl alcohol, and the mass ratio of film forming agent and solid electrolyte is 1:10~20；Positive electrode after cooling and the negative material for being coated with solid electrolyte are assembled into solid lithium ion battery.This method is simple, and energy consumption is small, at low cost.
Description
Technical field
The invention belongs to battery preparation technology field more particularly to a kind of preparation methods of solid lithium ion battery.
Background technology
Energy and environment are the primary conditions of the human society survival and development, are support nation-building and economic development
The two conflicting hang-ups that important substance basis and the current whole world are faced.With traditional non-regeneration energy
Constantly consumption and the worsening of global environment, utilization new green power are extremely urgent.Solar energy, wind energy, ocean
Energy, nuclear energy, biomass energy and Hydrogen Energy etc. are all the novel energies developed rapidly in recent years, they are in our daily lifes
Every field all play significant role.However in order to further improve the utilization ratio of the energy, must just be better achieved
The storage and conversion of the energy, green energy resource are a kind of novel renewable energies, it can realize well the energy storage conversion with
It utilizes.Wherein, it is the master for improving energy conversion and utilization ratio using lithium ion battery as the new green power technology of representative
Power army, with the rapid development of electronic electric industry, by extensive exploitation and application.
However, traditional lithium ion battery is still faced with many challenges, most important one is safety problem.It passes
The commercial Li-ion battery of system is generally using organic electrolyte system, and organic electrolyte is inflammable, volatile, easy-to-leak liquid, with
The increase of cycle-index, the Li dendrite of generation easily pierces through membrane and causes battery short circuit, so as to cause combustion explosion.It is although solidifying
Xanthan polymer electrolyte combines the high ionic conductivity of liquid electrolyte and the high safety of high rate performance and solid electrolyte
Property, solves the safety issue of lithium ion battery to a certain extent, but it uses liquid organic solvent as plasticizer,
Safety issue cannot be solved from source.In order to solve the safety problem of lithium ion battery from source, people are to all solid state
Lithium ion battery has carried out substantial amounts of research.At present, all-solid lithium-ion battery is in portable electronic product and microelectronic device
Etc., dosage is increasing, and the application in electric vehicle and large-scale energy storage equipment is also researched and developed extensively.
Solid ionic battery is mainly prepared using following scheme in the prior art：
1st, the collision process of magnetron sputtering method, i.e. incoming particle and target.Incoming particle undergoes complicated scattering in target
Part momentum, is transmitted to target atom by journey and target atom collision, this target atom cascaded again with the collision of other target atoms, formation
Journey.Enough momentum that target atom acquisition in this cascade process near some surfaces moves out, leave target and are sputtered out
Come.It in electronics under the action of electric field E, collides during substrate is flown to ar atmo, its ionization is made to produce Ar just
Ion and new electronics；New electronics flies to substrate, and Ar ions accelerate to fly to cathode target under electric field action, and are banged with high-energy
Target surface is hit, makes target that sputtering occur and forms film.To plus plate current-collecting body, positive electrode, solid electrolyte, negative material bears
Pole collector successively carries out Magnetron Sputtering Thin Film preparation, so as to obtain a complete solid-State Thin Film Li-Ion Batteries.This
The main problem of kind of method is：The utilization rate of target is not high, it is necessary to which large-scale instrument carries out magnetron sputtering, and cost is excessively high.
2nd, solid electrolyte piece construction from part first, carries out compression molding, and is obtained under certain condition by solid-phase synthesis
To solid electrolyte piece.Then, the positive active materials such as cobalt acid lithium are coated in the one side of electrolyte sheet, then by electrolyte sheet
In addition connect the negative materials such as lithium piece on one side, so as to be assembled into a complete all-solid lithium-ion battery.This method
Problem is：Traditional compression molding technology obtains the process flow very complicated of solid electrolyte piece and cost is higher, the cycle
Long, solid electrolyte piece is rigid, is realized by squeezing between positive electrode, negative material and solid electrolyte
Physical contact, the cell contact resistance of this method assembling is larger, and during cell reaction lithium ion and negative oxygen ion only layer with
Layer contact surface transfers, and battery polarization resistance is also larger.
3rd, gradient-structure construction from part, the preparation method are first to configure different component concentration or the anode of granularity or molecular weight
Anode sizing agent by the concentration gradient or granular gradient or molecular weight gradient of component is coated on collector and prepares electrode by slurry
Layer, then coats solid-state electrolyte layer on electrode layer, last adhesion metal negative electrode or configuration different component concentration or granularity
Or the negative electrode slurry of molecular weight, by concentration gradient or granular gradient opposite in the method for preparing anode electrode layer or molecular weight
Negative electrode slurry coating is prepared negative electrode layer by gradient on the electrolyte layer, and last adhesion collector is to get with gradient-structure
Solid lithium battery.The problem of this method is：Low production efficiency, the governing factor of technique is too many and more complicated, into
This height, the uniformity of product are not sufficiently stable.
The content of the invention
The present invention provides a kind of preparation method of solid lithium ion battery, it is intended to solve the above problems.
The present invention provides a kind of preparation method of solid lithium ion battery, the described method includes：
Solid electrolyte is placed in solvent and is disperseed, obtains solid electrolyte solution, wherein, solid electrolyte with
The mass ratio of solvent is 1:5~50；
Anode of the ternary material as solid lithium ion battery is chosen, lithium metal is as cathode；
Film forming agent, and the surface coated on anode and cathode are added in solid electrolyte solution, dry and will be applied
The anode for having covered solid electrolyte is sintered under conditions of 800~1000 DEG C, keeps the temperature 2~10h, is cooled down, wherein, film forming agent is
The mass ratio of polyvinylidene fluoride, polytetrafluoroethylene (PTFE) or polyvinyl alcohol, film forming agent and solid electrolyte is 1:10~20；
Positive electrode after cooling and the negative material for being coated with solid electrolyte are assembled into solid lithium ion battery.
The present invention provides a kind of preparation method of solid lithium ion battery, by adding in film forming agent in solid electrolyte,
And the surface coated in anode and cathode, so as to form integral structure, solid lithium ion that thus anode and cathode assemble
Battery has good interface contact performance and chemical property, compared with preparation method of lithium ion battery of the prior art,
Method is simple, and energy consumption is small, at low cost.
Specific embodiment
Goal of the invention, feature, advantage to enable the present invention is more apparent and understandable, below to of the invention real
The technical solution applied in example is clearly and completely described, it is clear that described embodiment is only that a present invention part is real
Apply example, and not all embodiments.Based on the embodiments of the present invention, those skilled in the art are not making creative work
Under the premise of all other embodiments obtained, belong to the scope of protection of the invention.
The present invention provides a kind of preparation method of solid lithium ion battery, and this method comprises the following steps：
Disperse Step 1: solid electrolyte is placed in solvent, obtain solid electrolyte solution, wherein, solid-state electricity
The mass ratio for solving matter and solvent is 1:5~50；
Step 2: choosing anode of the ternary material as solid lithium ion battery, lithium metal is as cathode；
Step 3: film forming agent is added in solid electrolyte solution, and the surface coated on anode and cathode, it is dry, with
And be sintered the anode for being coated with solid electrolyte under conditions of 800 DEG C -1000 DEG C, 2~10h is kept the temperature, is cooled down, wherein, into
Film is polyvinylidene fluoride, polytetrafluoroethylene (PTFE) or polyvinyl alcohol, and the molar ratio of film forming agent and solid electrolyte is 1:20~
30；
Step 4: by positive electrode after cooling and be coated with solid electrolyte negative material be assembled into solid-state lithium from
Sub- battery.
The embodiment of the present invention provides a kind of preparation method of solid lithium ion battery, by being added in solid electrolyte
Film forming agent, and the surface coated in anode and cathode, so as to form integral structure, what thus anode and cathode assembled consolidates
State lithium ion battery has good interface contact performance and chemical property, compared with lithium ion battery of the prior art
Preparation method, method is simple, and energy consumption is small, at low cost.
Specifically, in step 1, solid electrolyte is the powder as made from solid-phase synthesis, wherein, solid electrolyte is
Inorganic solid electrolyte or solid polyelectrolyte.Inorganic solid electrolyte can be the substance of below formula
Li3xLa2/3-xTiO3,A3B2Si3O12, A cations and B cations are eight-coordinate and hexa-coordinate respectively, Li5La3M2O12(M=Nb
Or Ta), Li6ALa2M2O12(A=Ca, Sr or Ba；M=Nb or Ta), Li5.5La3M1.75B0.25O12(M=Nb or Ta；B=In or
) and cubic system Li Zr7La3Zr2O12And Li7.06M3Y0.06Zr1.94O12(M=La, Nb or Ta).Solid polyelectrolyte can
Think PEO, PAN, PMMA, PVC or PVDF etc..The powder of solid electrolyte is dissolved in solvent and is stirred, is disperseed
Uniform solid electrolyte solution.Used solvent is N-Methyl pyrrolidone or any one of ethyl alcohol or acetone.
Specifically, in step 2, the ternary material of selection can be cobalt nickel lithium manganate ternary material or cobalt acid lithium, manganese
The mixing material of sour lithium and LiFePO4.
Specifically, in step 3, film forming agent is added in solid electrolyte solution, and by way of spin coating or printing
Surface coated on anode and cathode, to form the electrolytic thin-membrane with certain mechanical strength in anode and negative terminal surface.
Preferably, film forming agent is polyvinylidene fluoride, and the molar ratio of film forming agent and solid electrolyte is 1:20.
Preferably, the anode for being coated with solid electrolyte is subjected to high temperature sintering, wherein, it is 2-5 to control heating rate
DEG C/min, heating temperature is 900 DEG C, and 7~9h is kept the temperature after sintering.
Embodiment 1
1st, using solid-phase synthesis composite solid state electrolyte powder, 10g Li are taken5La3Ta2O12It is dissolved in 50gN- methylpyrroles
Disperseed in alkanone, be uniformly dispersed, without solid electrolyte solution existing for powder.
2nd, 1g polyvinylidene fluoride is added in solid electrolyte solution, after stirring evenly, is spun on block LiFePO4
Material and reguline metal lithium surface, and be dried.
3rd, the LiFePO 4 material for being coated with solid electrolyte is placed in Muffle furnace, it is 2 to control heating rate
DEG C/min, the temperature of Muffle furnace is made to be increased to 800 DEG C, and 2h is kept the temperature, furnace cooling is taken out spare.
4th, the negative material that the positive electrode and step 2 step 3 being prepared are prepared is assembled into solid lithium ion
Battery.
Embodiment 2
1st, using solid-phase synthesis composite solid state electrolyte powder, 10g Li are taken5La3Ta2O12It is dissolved in 100gN- methyl pyrroles
Disperseed in pyrrolidone, be uniformly dispersed, without solid electrolyte solution existing for powder.
2nd, 0.5g polyvinylidene fluoride is added in solid electrolyte solution, after stirring evenly, is spun on block ferric phosphate
Lithium material and reguline metal lithium surface, and be dried.
3rd, the LiFePO 4 material for being coated with solid electrolyte is placed in Muffle furnace, it is 2 to control heating rate
DEG C/min, the temperature of Muffle furnace is made to be increased to 800 DEG C, and 2h is kept the temperature, furnace cooling is taken out spare.
4th, the negative material that the positive electrode and step 2 step 3 being prepared are prepared is assembled into solid lithium ion
Battery.
Embodiment 3
1st, using solid-phase synthesis composite solid state electrolyte powder, 10g Li are taken5La3Ta2O12Be dissolved in 500g ethyl alcohol into
Row is scattered, is uniformly dispersed, without solid electrolyte solution existing for powder.
2nd, 0.5g polytetrafluoroethylene (PTFE) is added in solid electrolyte solution, after stirring evenly, is spun on block LiFePO4
Material and reguline metal lithium surface, and be dried.
3rd, the LiFePO 4 material for being coated with solid electrolyte is placed in Muffle furnace, it is 5 to control heating rate
DEG C/min, the temperature of Muffle furnace is made to be increased to 1000 DEG C, and 5h is kept the temperature, furnace cooling is taken out spare.
4th, the negative material that the positive electrode and step 2 step 3 being prepared are prepared is assembled into solid lithium ion
Battery.
Embodiment 4
1st, using solid-phase synthesis composite solid state electrolyte powder, 10g Li are taken5La3Ta2O12Be dissolved in 200g ethyl alcohol into
Row is scattered, is uniformly dispersed, without solid electrolyte solution existing for powder.
2nd, 1g polytetrafluoroethylene (PTFE) is added in solid electrolyte solution, after stirring evenly, is spun on block LiFePO4 material
Material and reguline metal lithium surface, and be dried.
3rd, the LiFePO 4 material for being coated with solid electrolyte is placed in Muffle furnace, it is 5 to control heating rate
DEG C/min, the temperature of Muffle furnace is made to be increased to 1000 DEG C, and 5h is kept the temperature, furnace cooling is taken out spare.
4th, the negative material that the positive electrode and step 2 step 3 being prepared are prepared is assembled into solid lithium ion
Battery.
Embodiment 5
1st, using solid-phase synthesis composite solid state electrolyte powder, 10g Li are taken5La3Ta2O12Be dissolved in 250g acetone into
Row is scattered, is uniformly dispersed, without solid electrolyte solution existing for powder.
2nd, 0.75g polyvinyl alcohol is added in solid electrolyte solution, after stirring evenly, is spun on block LiFePO4
Material and reguline metal lithium surface, and be dried.
3rd, the LiFePO 4 material for being coated with solid electrolyte is placed in Muffle furnace, it is 3 to control heating rate
DEG C/min, the temperature of Muffle furnace is made to be increased to 900 DEG C, and 5h is kept the temperature, furnace cooling is taken out spare.
4th, the negative material that the positive electrode and step 2 step 3 being prepared are prepared is assembled into solid lithium ion
Battery.
Embodiment 6
1st, using solid-phase synthesis composite solid state electrolyte powder, 10g Li are taken5La3Ta2O12Be dissolved in 250g acetone into
Row is scattered, is uniformly dispersed, without solid electrolyte solution existing for powder.
2nd, 0.5g polyvinyl alcohol is added in solid electrolyte solution, after stirring evenly, is spun on block LiFePO4 material
Material and reguline metal lithium surface, and be dried.
3rd, the LiFePO 4 material for being coated with solid electrolyte is placed in Muffle furnace, it is 3 to control heating rate
DEG C/min, the temperature of Muffle furnace is made to be increased to 900 DEG C, and 5h is kept the temperature, furnace cooling is taken out spare.
4th, the negative material that the positive electrode and step 2 step 3 being prepared are prepared is assembled into solid lithium ion
Battery.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of solid lithium ion battery, which is characterized in that the described method includes：
Solid electrolyte is placed in solvent and is disperseed, obtains solid electrolyte solution, wherein, solid electrolyte and solvent
Mass ratio is 1:5~50；
Anode of the ternary material as solid lithium ion battery is chosen, lithium metal is as cathode；
Film forming agent, and the surface coated on anode and cathode are added in solid electrolyte solution, dry and will be coated with solid
The anode of state electrolyte is sintered under conditions of 800~1000 DEG C, keeps the temperature 2~10h, is cooled down, wherein, film forming agent is to gather inclined difluoro
The mass ratio of ethylene, polytetrafluoroethylene (PTFE) or polyvinyl alcohol, film forming agent and solid electrolyte is 1:10~20；
Positive electrode after cooling and the negative material for being coated with solid electrolyte are assembled into solid lithium ion battery.
2. according to the method described in claim 1, it is characterized in that, ternary material is cobalt nickel lithium manganate ternary material or cobalt acid
The mixing material of lithium, LiMn2O4 and LiFePO4.
3. according to the method described in claim 1, it is characterized in that, solvent is in N-Methyl pyrrolidone or ethyl alcohol or acetone
It is any.
4. according to the method described in claim 1, it is characterized in that, the heating rate of sintering is 2-5 DEG C/min.
5. according to the method described in claim 1, it is characterized in that, the temperature of sintering is 900 DEG C.
6. according to the method described in claim 1, it is characterized in that, the time of heat preservation is 7~9h.
7. according to the method described in claim 1, it is characterized in that, using the method for spin coating or printing coat.
8. according to the method described in claim 1, it is characterized in that, the mass ratio of solid electrolyte and solvent is 1:5~20.
9. according to claim 1~8 any one of them method, which is characterized in that solid electrolyte is inorganic solid electrolyte
Or solid polyelectrolyte.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111162244A (en) * | 2019-12-25 | 2020-05-15 | 浙江锋锂新能源科技有限公司 | Method for obtaining ultrathin solid electrolyte on surface of metal lithium and prepared assembly |
| CN111276736A (en) * | 2020-02-06 | 2020-06-12 | 哈尔滨工业大学 | Method for co-sintering positive electrode, electrolyte and inorganic lithium salt |
| CN111525181A (en) * | 2020-05-08 | 2020-08-11 | 上海空间电源研究所 | All-solid-state battery with low interface resistance and preparation method thereof |
| CN112331827A (en) * | 2020-10-27 | 2021-02-05 | 五邑大学 | Large-current in-situ carbonization method for solid electrolyte anode |
| CN112582666A (en) * | 2019-09-27 | 2021-03-30 | 荣盛盟固利新能源科技有限公司 | Bipolar lithium ion battery and preparation method thereof |
| CN112993410A (en) * | 2021-02-09 | 2021-06-18 | 深圳市齐得隆电子有限公司 | Manufacturing method of novel high-capacity solid-state lithium ion battery |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112582666A (en) * | 2019-09-27 | 2021-03-30 | 荣盛盟固利新能源科技有限公司 | Bipolar lithium ion battery and preparation method thereof |
| CN111162244A (en) * | 2019-12-25 | 2020-05-15 | 浙江锋锂新能源科技有限公司 | Method for obtaining ultrathin solid electrolyte on surface of metal lithium and prepared assembly |
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| CN112331827A (en) * | 2020-10-27 | 2021-02-05 | 五邑大学 | Large-current in-situ carbonization method for solid electrolyte anode |
| CN112993410A (en) * | 2021-02-09 | 2021-06-18 | 深圳市齐得隆电子有限公司 | Manufacturing method of novel high-capacity solid-state lithium ion battery |
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Application publication date: 20180601 |