CN105098227B - All-solid lithium-ion battery and preparation method thereof - Google Patents
All-solid lithium-ion battery and preparation method thereof Download PDFInfo
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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
- 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
- H01M10/058—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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
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- 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
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Abstract
The invention discloses a kind of all-solid lithium-ion battery and preparation method thereof, all-solid lithium-ion battery is prepared using inkjet technology, different component dissolving is prepared into slurry in a solvent, it is placed among different print cartridges, use computer programming, longitudinal stepwise gradient printing electrode and electrolyte, electrolyte longitudinal gradient change in electrode plates, gradient-structure distribution of the electrolyte in pole piece can reduce the interface impedance of electrode active material/electrolyte, conducted beneficial to the depth of lithium ion, the capacity property of maximum performance active material；All-solid lithium-ion battery structure prepared by inkjet printing, in addition to collector, other parts turn into the lamination of an entirety, and each component is in close contact, is regularly arranged in the structure of the lamination, and interface impedance is well below the mechanical all-solid lithium-ion battery for laminating mode and preparing.The mode of the inkjet printing is convenient and swift, is adapted to large-scale production.
Description
Technical field
The present invention relates to a kind of preparation technology of lithium ion battery, more particularly to a kind of all-solid lithium-ion battery and its
The technique for preparing all-solid lithium-ion battery using inkjet printing.
Background technology
All-solid lithium-ion battery is as accumulation power supply of future generation, because it has high energy density, good mechanicalness
Can, excellent electrochemical stability and nonflammable advantage and receive more and more attention.All-solid lithium-ion battery
Structure is similar to traditional liquid electrolyte lithium ion battery, is mainly made up of both positive and negative polarity and solid electrolyte, solid electrolyte
It is divided into inorganic solid electrolyte and organic solid-state electrolyte, inorganic solid electrolyte room temperature lithium ion conductivity is high, cryogenic property
It is good, but interface stability is poor；Organic solid-state electrolyte is made up of polymeric substrates and inorganic lithium salt, lithium ion conductivity under high temperature
It is higher, be not suitable for discharge and recharge under low temperature.Electrode/electrolyte interface problem is institute face in solid lithium ion battery evolution at present
The subject matter faced, the exposure level of two-phase interface have a significant impact to the overall performance of battery.It is high by being coated in interface
The binding agent of electric conductivity or hot pressing or it is integral sintered can reduce the problem of interracial contact is bad to a certain extent, but technique compared with
For complexity, be not suitable for large-scale production.
The content of the invention
It is an object of the invention to provide a kind of all-solid lithium-ion battery and preparation method thereof, uses inkjet printing mode system
Standby all-solid lithium-ion battery has high security performance, big volume energy density and mass energy density and good
The advantages that cyclical stability.
The purpose of the present invention is achieved through the following technical solutions：
A kind of all-solid lithium-ion battery, it is made up of positive pole, negative pole, solid electrolyte film layer, wherein：The positive pole is by just
Pole collector, positive active material, inorganic nano-filler and solid electrolyte are formed, doping of the inorganic nano-filler in positive pole
Measure and be laterally away from plus plate current-collecting body side from close to plus plate current-collecting body one for 5-15wt.%, doping of the solid electrolyte in positive pole
To reducing in gradient, from positive active material/plus plate current-collecting body contact interface to positive pole/solid electrolyte film layer contact interface electricity
The doping of solution matter reduces in gradient from 50wt.% to 10wt.%；The negative pole is by negative current collector, negative electrode active material, inorganic
Nano filling and solid electrolyte are formed, and doping of the inorganic nano-filler in negative pole is 5-15wt.%, and solid electrolyte exists
Doping in negative pole is laterally away from negative current collector direction from close negative current collector one and reduced in gradient, from negative electrode active material
Matter/negative current collector contact interface to the doping of negative pole/solid electrolyte film layer contact interface electrolyte from 50wt.% to
10wt.% reduces in gradient；The solid electrolyte film layer is made up of solid electrolyte and inorganic nano-filler, and inorganic nano is filled out
Expect that the content in solid electrolyte film layer is 10-20wt.%
A kind of method that inkjet printing prepares above-mentioned all-solid lithium-ion battery, comprises the following steps：
First, positive active material, inorganic nano-filler, negative electrode active material and solid electrolyte are dissolved in solvent respectively
In be prepared into slurry；
2nd, different component slurry is subjected to print cartridge packing using ink-jet printer；
3rd, controlled by computer programming, the positive active material of longitudinal direction classification inkjet printing all-solid lithium-ion battery,
Inorganic nano-filler, solid electrolyte, negative electrode active material；
4th, both positive and negative polarity collector coating is obtained or by print structure mechanical stitch and collector knot using physical vapour deposition (PVD)
It is combined, prepares all-solid lithium-ion battery.
In the present invention, solid electrolyte and the electrolysis material in solid electrolyte film layer adulterated in both positive and negative polarity active material
Expect for same material.
In the present invention, all parts are obtained by inkjet printing in addition to collector in gained battery structure, and each several part is close
Contact, the page order of both positive and negative polarity can be adjusted as needed.
In the present invention, different component slurry is divided in different print cartridges during inkjet printing in gained battery structure
Central, the gradient distribution of each component in the vertical is controlled by computer programming.
In the present invention, compound positive and negative pole material and solid electrolyte are obtained by the way of longitudinal stepwise gradient inkjet printing
The doping of film layer, wherein solid electrolyte in pole piece is laterally away from collector direction from close collector one and subtracted in gradient
It is small, from electrode active material/collector contact interface to the doping of electrode/electrolyte film layer contact interface electrolyte from
50wt.% to 10wt.% reduces in gradient, and the variable gradient of electrolyte doping determines according to the thickness of inkjet printing electrode.
In the present invention, the positive active material is cobalt acid lithium, LiMn2O4, LiFePO4, lithium nickelate, nickel ion doped, five
Any one in V 2 O, nickel-cobalt-manganese ternary material；Negative electrode active material be carbon-based material, silica-base material, tin-based material,
Any one in lithium titanate.
In the present invention, the solid electrolyte film layer includes inorganic compounding solid electrolyte and organic composite polymeric thing solid-state
At least one of electrolyte；Wherein, inorganic solid electrolyte includes oxide system solid electrolyte, sulfide-based solid state electrolysis
Matter, LiPON, Li3At least one of N；Organic polymer solid electrolyte includes PEO bases solid electrolyte, PAN bases solid-state electricity
Xie Zhi, PMMA base solid electrolyte, PVDF bases solid electrolyte, PEO-PAN bases solid electrolyte, PEO-PMMA base solid state electrolysises
Matter, PEO-PVDF bases solid electrolyte, PMMA-PVDF bases solid electrolyte, PMMA-PAN bases solid electrolyte, PAN-PVDF bases
Solid electrolyte, PEO-PAN-PMMA bases solid electrolyte, PEO-PVDF-PMMA bases solid electrolyte, PEO-PAN-PVDF bases
At least one of solid electrolyte, PAN-PMMA-PVDF base solid electrolytes.The solid-state in all-solid lithium-ion battery structure
While electrolyte membrane layer serves as electrolyte conducts lithium ion, used as barrier film and prevent electronic conduction, and be avoided that positive and negative
The contact short circuit of pole.The mechanical performance that electrolyte has had, thickness can be controlled at 10-500 μm.
In the present invention, the inorganic nano-filler includes α-Al2O3、SiO2、TiO2、BaTiO3, in MOF, ZIF series extremely
Few one kind；By inkjet technology, inorganic nano-filler may be uniformly dispersed among whole battery system；Inorganic nano is filled out
The addition of material can strengthen the mechanical strength of solid electrolyte, increase the electrical conductivity of solid electrolyte, inorganic in electrode material to receive
The addition of rice filler can also improve the interface compatibility of solid electrolyte/active material；In addition, organic polymer-based
The addition of Nano filling can also reduce the crystallinity of polymer in solid electrolyte, improve ionic conductivity.Wherein, it is inorganic to receive
Doping of the rice filler in positive and negative electrode is 5-15wt.%, and the doping in solid electrolyte film layer is 10-20wt.%.
In the present invention, the plus plate current-collecting body, negative current collector can be by physical vapour deposition (PVD)s（Vacuum evaporation or magnetic control splash
Penetrate）Method obtains, and the electron conduction that gained coating has had, is contacted with electrode material atomic level, its thickness can control
Below 1 μm, the volume energy density and mass energy density of all-solid lithium-ion battery can be greatly lifted；It can also lead to
The mode of mechanical stitch overlaps together inkjet printing laminated construction and both positive and negative polarity collector, and technique is simple, is adapted to scale
Production.
Inkjet technology is used mainly as office equipment till now, and inkjet technology system is used in the present invention
Standby all-solid lithium-ion battery, different component dissolving is prepared into slurry in a solvent, is placed among different print cartridges, uses electricity
Brain programming, longitudinal stepwise gradient printing electrode and electrolyte, electrolyte longitudinal gradient change, electrolyte in electrode plates
Gradient-structure distribution in pole piece can reduce the interface impedance of electrode active material/electrolyte, beneficial to the depth of lithium ion
Conduction, the capacity property of maximum performance active material；All-solid lithium-ion battery structure prepared by inkjet printing, except collector
In addition, other parts turn into the lamination of entirety, in the structure of the lamination each component be in close contact, regularly arranged, boundary
Face impedance is well below the mechanical all-solid lithium-ion battery for laminating mode and preparing.The mode of the inkjet printing is convenient and swift, suitable
Close large-scale production.
Brief description of the drawings
Fig. 1 is that inkjet printing prepares all-solid lithium-ion battery structural representation；
Fig. 2 is that soldering polar ear post package is soft-package battery schematic diagram；
Fig. 3 is battery charging and discharging loop test curve；
Fig. 4 is circulating battery volt-ampere curve.
Embodiment
Technical scheme is further described below in conjunction with the accompanying drawings, but is not limited thereto, it is every to this
Inventive technique scheme is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, all should cover
In protection scope of the present invention.
Embodiment 1
As shown in figure 1, inkjet printing all-solid lithium-ion battery is by plus plate current-collecting body 1, negative current collector 6, inorganic nano
Filler 3, solid electrolyte film layer 4, solid electrolyte particle 7, positive active material 2, negative electrode active material 5 are formed, and are sprayed successively
Each construction unit of ink printing all-solid lithium-ion battery, content becomes solid electrolyte in gradient on longitudinal direction in both positive and negative polarity
Change.
Embodiment 2
In ink jet printing process, solid electrolyte longitudinal gradient distribution on electrode:From close to collector side
50wt.% reduces to the 10wt.% gradients close to intermediate solid-state electrolyte film layer side, and the gradient distribution on longitudinal direction can be at utmost
Reduction interface impedance, be advantageous to the migration of lithium ion, improve all-solid lithium-ion battery chemical property, under the graded
The capacity property of active material can farthest be played.
Embodiment 3
Inkjet printing combination physical vapour deposition (PVD) prepares all-solid lithium-ion battery, and positive active material uses lithium nickelate,
Negative electrode active material uses lithium titanate, PEO-LiClO4- TiO2Electrolyte is as solid electrolyte film material, TiO2As nothing
Machine filler, DMF prepare the slurry of each component, ink-jet time of the computer design each component in print procedure on longitudinal direction as solvent
And order, it is 5wt.% to control doping of the inorganic nano-filler in positive and negative electrode, the doping in solid electrolyte film layer
For 10wt.%, solid electrolyte membrane thickness degree is 100 μm；Vacuum evaporation technology is used after each component is fully dried, in positive pole
Side vacuum evaporated aluminium collector coating, negative pole side vacuum evaporation copper current collector coating, it is 1 to control positive and negative afflux body thickness
μm.After soldering polar ear, Soft Roll encapsulation, electro-chemical test is carried out.Gained soft-package battery is prepared as shown in Fig. 2 soft-package battery thickness
About 3mm.All-solid lithium-ion battery charge and discharge cycles test curve is understood obtained by inkjet printing as shown in Figure 3,0.1c multiplying powers
Lower 20 capacity retention rates of circulation are 96.5%.
Embodiment 4
Cyclic voltammetry curve test, sweep speed 0.05mV/s, as shown in figure 4, the redox of battery are carried out to battery
Spike potential is corresponding with battery charging and discharging platform, no miscellaneous peak, i.e. the generation without side reaction, also provides guarantor for battery long circulating
Card.
Embodiment 5
The present embodiment is as different from Example 3：Positive active material uses cobalt acid lithium, and negative electrode active material uses thick
Silicon, LiPON electrolyte is as solid electrolyte film material, α-Al2O3As inorganic filler, inorganic nano-filler is in positive negative electricity
Doping in extremely is 8wt.%, and the doping in solid electrolyte film layer is 12wt.%, and solid electrolyte membrane thickness degree is
150 μm, afflux body thickness is 750nm.
Embodiment 6
The present embodiment is as different from Example 3：Positive active material uses LiMn2O4, and negative electrode active material uses stone
Ink, P（EO-MMA）-LiTFSI- SiO2Electrolyte is as solid electrolyte film material, SiO2It is inorganic to receive as inorganic filler
Doping of the rice filler in positive and negative electrode is 10wt.%, and the doping in solid electrolyte film layer is 20wt.%, and solid-state is electric
It is 50 μm to solve matter thicknesses of layers, and vacuum evaporation collector thickness of coating is 500nm.
Claims (10)
1. a kind of all-solid lithium-ion battery, it is made up of positive pole, negative pole, solid electrolyte film layer, it is characterised in that the positive pole
It is made up of plus plate current-collecting body, positive active material, inorganic nano-filler and solid electrolyte, inorganic nano-filler is in positive pole
Doping is 5-15wt.%, from positive active material/plus plate current-collecting body contact interface to positive pole/solid electrolyte film layer contact circle
The doping of face solid electrolyte reduces in gradient from 50wt.% to 10wt.%；The negative pole is by negative current collector, negative electrode active
Material, inorganic nano-filler and solid electrolyte are formed, and doping of the inorganic nano-filler in negative pole be 5-15wt.%, from bearing
Doping of the pole active material/negative current collector contact interface to negative pole/solid electrolyte film layer contact interface solid electrolyte
Reduce in gradient from 50wt.% to 10wt.%；The solid electrolyte film layer is made up of solid electrolyte and inorganic nano-filler,
Content of the inorganic nano-filler in solid electrolyte film layer is 10-20wt.%.
2. all-solid lithium-ion battery according to claim 1, it is characterised in that the positive active material be cobalt acid lithium,
Any one in LiMn2O4, LiFePO4, lithium nickelate, nickel ion doped, vanadic anhydride, nickel-cobalt-manganese ternary material.
3. all-solid lithium-ion battery according to claim 1, it is characterised in that the negative electrode active material is carbon substrate
Any one in material, silica-base material, tin-based material, lithium titanate.
4. all-solid lithium-ion battery according to claim 1, it is characterised in that the solid electrolyte film layer includes nothing
At least one of machine composite solid electrolyte and organic composite polymeric thing solid electrolyte.
5. all-solid lithium-ion battery according to claim 4, it is characterised in that the inorganic compounding solid electrolyte bag
Include oxide system solid electrolyte, sulfide-based solid electrolyte, LiPON, Li3At least one of N.
6. all-solid lithium-ion battery according to claim 4, it is characterised in that the organic composite polymeric thing solid-state electricity
Solve matter include PEO bases solid electrolyte, PAN bases solid electrolyte, PMMA bases solid electrolyte, PVDF bases solid electrolyte,
PEO-PAN bases solid electrolyte, PEO-PMMA bases solid electrolyte, PEO-PVDF bases solid electrolyte, PMMA-PVDF base solid-states
Electrolyte, PMMA-PAN bases solid electrolyte, PAN-PVDF bases solid electrolyte, PEO-PAN-PMMA bases solid electrolyte,
PEO-PVDF-PMMA bases solid electrolyte, PEO-PAN-PVDF bases solid electrolyte, PAN-PMMA-PVDF base solid electrolytes
At least one of.
7. all-solid lithium-ion battery according to claim 1, it is characterised in that the thickness of the solid electrolyte film layer
Control is at 10-500 μm.
8. all-solid lithium-ion battery according to claim 1, it is characterised in that the inorganic nano-filler include α-
Al2O3、SiO2、TiO2、BaTiO3At least one of series.
9. all-solid lithium-ion battery according to claim 1, it is characterised in that the plus plate current-collecting body, negative current collector
Thickness control below 1 μm.
10. a kind of method that inkjet printing prepares all-solid lithium-ion battery described in claim 1-9 any claims, it is special
Sign is that methods described step is as follows：
First, positive active material, inorganic nano-filler, negative electrode active material and solid electrolyte are dissolved respectively and made in a solvent
It is standby into slurry；
2nd, different component slurry is subjected to print cartridge packing using ink-jet printer；
3rd, controlled by computer programming, longitudinal direction is classified the positive active material, inorganic of inkjet printing all-solid lithium-ion battery
Nano filling, solid electrolyte, negative electrode active material；
4th, both positive and negative polarity collector coating is obtained using physical vapour deposition (PVD) or is incorporated in print structure mechanical stitch and collector
Together, all-solid lithium-ion battery is prepared.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE102016212293A1 (en) * | 2016-07-06 | 2018-01-11 | Robert Bosch Gmbh | Method for producing a cathode, cathode and battery cell |
| CN106654367B (en) * | 2016-12-19 | 2020-11-24 | 天津力神电池股份有限公司 | Method for preparing electrolyte membrane and solid lithium battery |
| JP6662802B2 (en) * | 2017-02-27 | 2020-03-11 | 国立大学法人北陸先端科学技術大学院大学 | Oxide all solid state battery |
| CN107394272A (en) * | 2017-06-20 | 2017-11-24 | 哈尔滨工业大学无锡新材料研究院 | A kind of solid lithium ion battery and preparation method thereof |
| CN107565090A (en) * | 2017-08-30 | 2018-01-09 | 清陶（昆山）能源发展有限公司 | A kind of positive plate of lithium battery and preparation method thereof |
| CN107731542B (en) * | 2017-10-17 | 2019-12-03 | 中国科学院青岛生物能源与过程研究所 | A kind of solid state battery capacitor |
| CN108232318B (en) * | 2018-01-30 | 2020-07-17 | 陕西煤业化工技术研究院有限责任公司 | Manufacturing method of all-solid-state power lithium ion battery |
| CN108258323B (en) * | 2018-01-30 | 2019-09-10 | 陕西煤业化工技术研究院有限责任公司 | A kind of production method of high specific energy solid lithium battery |
| CN110224107A (en) * | 2018-03-02 | 2019-09-10 | 上海汽车集团股份有限公司 | A kind of solid state battery electrode and preparation method thereof and a kind of solid state battery |
| CN108933258A (en) * | 2018-06-27 | 2018-12-04 | 淄博火炬能源有限责任公司 | The preparation method of the all-solid lithium-ion battery of three-dimensional composition metal cathode of lithium |
| CN111435761B (en) * | 2019-01-11 | 2021-08-10 | 荣盛盟固利新能源科技有限公司 | All-solid-state lithium ion battery and hot-pressing preparation method of multilayer electrolyte membrane thereof |
| CN109786812B (en) * | 2019-01-15 | 2021-01-29 | 北京理工大学 | Photocuring solid composite electrolyte and preparation method thereof |
| CN109786817B (en) * | 2019-01-23 | 2021-09-21 | 蜂巢能源科技有限公司 | Solid lithium battery, application thereof and method for preparing non-woven fabric reinforced solid electrolyte membrane |
| CN110120509B (en) * | 2019-05-23 | 2021-01-12 | 桑德新能源技术开发有限公司 | All-solid-state battery and preparation method thereof |
| CN110165303B (en) * | 2019-06-10 | 2022-04-26 | 南京理工大学北方研究院 | Secondary battery, preparation method thereof and electric equipment |
| CN110350238A (en) * | 2019-07-03 | 2019-10-18 | 中兴高能技术有限责任公司 | A kind of all-solid lithium-ion battery and preparation method thereof with porous gradient-structure |
| CN110380133A (en) * | 2019-08-02 | 2019-10-25 | 中南大学 | A kind of transition zone design method of inorganic solid electrolyte and positive interpolar |
| CN111864272B (en) * | 2020-06-09 | 2022-04-26 | 江苏大学 | High-safety volume energy density quasi-solid lithium ion battery and manufacturing method thereof |
| CN111092261B (en) * | 2019-12-12 | 2021-04-02 | 中国第一汽车股份有限公司 | Solid-state battery electrode unit |
| CN111509291A (en) * | 2020-04-15 | 2020-08-07 | 合肥工业大学 | Composite solid electrolyte membrane and preparation method and application thereof |
| CN114464766B (en) * | 2020-11-09 | 2024-05-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Novel negative electrode structure, preparation method thereof and battery |
| CN113675403A (en) * | 2021-07-30 | 2021-11-19 | 华南师范大学 | Solid-state battery and preparation method and application thereof |
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| JP4055671B2 (en) * | 2003-07-31 | 2008-03-05 | 日産自動車株式会社 | Non-aqueous electrolyte battery |
| JP5333184B2 (en) * | 2009-03-16 | 2013-11-06 | トヨタ自動車株式会社 | All solid state secondary battery |
| JP2011065982A (en) * | 2009-08-18 | 2011-03-31 | Seiko Epson Corp | Lithium battery electrode body and lithium battery |
| CN102738510B (en) * | 2012-06-25 | 2014-11-05 | 中南大学 | Solid electrolyte for lithium ion battery and application thereof |
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