CN108808080A - Nano-composite gel electrolyte, lithium secondary battery and preparation method thereof - Google Patents
Nano-composite gel electrolyte, lithium secondary battery and preparation method thereof Download PDFInfo
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- CN108808080A CN108808080A CN201810878168.0A CN201810878168A CN108808080A CN 108808080 A CN108808080 A CN 108808080A CN 201810878168 A CN201810878168 A CN 201810878168A CN 108808080 A CN108808080 A CN 108808080A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of electrolyte
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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
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Abstract
The present invention relates to a kind of nano-composite gel electrolytes, lithium secondary battery and preparation method thereof, the gel electrolyte is the introducing hydrophobically modified nano-particle in liquid electrolyte, and forming three-dimensional network with the intermolecular hydrogen bond action of electrolyte solvent by hydrophobically modified nano-particle and its surface-modified molecules makes Liquid Electrolyte Gels.The ionic conductivity of the gel electrolyte is close with same type electrolyte, and about 10‑3S/cm.The addition of hydrophobically modified nano-particle can effectively improve the lithium ion transference number of electrolyte, and reduce the interface impedance between electrolyte and lithium metal.In addition, compared with the pure electrolyte of same type, there are preferably compatibility and cyclical stability between the gel electrolyte and metal lithium electrode.The gel electrolyte can be by being directly coated with or the method for swelling of paint coating is combined on diaphragm, and preparation process is simple, easy to produce.
Description
Technical field
The present invention relates to lithium metal secondary cell fields, and in particular to a kind of nano-composite gel electrolyte, the secondary electricity of lithium
Pond and preparation method thereof.
Background technology
With the development of society, environmental protection and energy saving have been to be concerned by more and more people.Lithium ion battery is because having higher energy
Metric density, longer cycle life and lower environment influence to become most popular one of chemical energy source.Lithium ion battery pair
Daily life produces far-reaching influence, and commercially use Carbon anode lithium ion battery is substantially close to its theory
Capacity, it is difficult to meet mancarried electronic aid, electric vehicle and extensive energy stores etc. higher and higher application requirement.Cause
This, still there is an urgent need to energy density higher, the higher batteries of safety.
Lithium metal has maximum theoretical energy density（3860 mAh/g）With minimum electrochemical potential（Relative to standard hydrogen
Electrode is 3.04 V）.Therefore, lithium metal battery is one of most potential next-generation energy storing devices, disclosure satisfy that highly energy-consuming
The demand of equipment.But when lithium metal is still had larger problem directly as battery cathode use.These problems include：
Cycle and high rate performance are poor, and safety is difficult to ensure.The main reason is that pole is not in currently used electrolyte for lithium metal
To stablize, the big polarization and highfield under high magnification lead to dendritic growth, and common diaphragm mechanical strength is relatively low to be easy to be pierced,
Therefore a series of safety issue can be caused.And substitute liquid electrolyte not with the solid electrolyte with higher force intensity
The deficiency of liquid electrolyte is only overcome, also provides possibility to develop new chemical cell.However, solid electrolyte and electricity
It contacts poor between pole, will produce larger interface resistance, this is unfavorable for the performance for playing solid electrolyte.
Invention content
The present invention in view of the above problems, provide nano-composite gel electrolyte and its lithium secondary battery and preparation method thereof,
The gel electrolyte has high ionic conductivity and positive and negative anodes compatibility is good, can effectively improve lithium battery cycle life, and nanometer is multiple
Solid electrolyte and interelectrode interface impedance can be reduced by closing gel.
Realize the technical scheme is that：A kind of nano-composite gel electrolyte, nano-composite gel electrolyte is by dredging
Water modified Nano particle and electrolyte form, and the mass fraction of hydrophobically modified nano-particle is 3- in nano-composite gel electrolyte
30%, for being spaced between battery diaphragm and positive and negative electrode.
The hydrophobically modified nano-particle is nanometer Al2O3, Nano-meter SiO_22, nano-ZnO, nano SnO2Or nano-TiO2Extremely
The size of few one kind, the hydrophobically modified nano-particle is 5-500 nm.
The hydrophobically modified nano-particle is modified nano-particle using silane coupling agent, and the silane coupling agent is
Hexamethyldisiloxane, dimethyl silicone polymer, dimethyl siloxane, octamethylcy-clotetrasiloxane, Trichloromethyl silane, two
One or more of dimethyl dichlorosilane (DMCS), methyl allyl acyloxypropyl trimethoxysilane.
Method of modifying is：By nano-particle and silane coupling agent ultrasonic disperse in ethyl alcohol, nano-particle and silane coupled
The mass fraction of agent in ethanol is respectively 1 ~ 10% and 1 ~ 15%, stirs 3 ~ 12 h under the conditions of 60 ~ 90 DEG C, uses centrifugation or mistake
Filter mode separation product is finally dried in vacuo with ethyl alcohol washed product.
The electrolyte includes lithium salts and organic solvent I, and the lithium salts is LiClO4、LiPF6、LiOH、LiTFSI、LiFSI
Or the one or more of LiFNFSI；The organic solvent I is propene carbonate, ethylene carbonate, dimethyl carbonate, carbonic acid two
One or more of ethyl ester, methyl ethyl carbonate or methyl propyl carbonate.
The lithium secondary battery includes anode pole piece, cathode pole piece, diaphragm and nano-composite gel electrolyte, the nanometer
Composite gel electrolyte is made of hydrophobically modified nano-particle and electrolyte, for being spaced between battery diaphragm and positive and negative electrode.
A kind of lithium secondary battery, structure include：Anode pole piece comprising plus plate current-collecting body and positive active material；It is negative
Pole pole piece comprising negative current collector and negative electrode active material；Diaphragm；Nano-composite gel electrolyte, be used to be spaced in every
Between film and anode pole piece and cathode pole piece.
Anode pole piece is that positive active material is coated on aluminium foil to obtain, and the positive active material is nickel cobalt aluminium ternary
Material, nickel-cobalt-manganese ternary material, cobalt acid lithium, lithium nickelate, LiMn2O4, LiFePO4 or phosphorus, sulphur, more lithium sulfides.
Cathode pole piece is that negative electrode active material is compound on copper foil to obtain, and the negative electrode active material is lithium metal, institute
It is plating or roll-in to state complex method.
Diaphragm can be porous PE films, porous PP/PE/PP composite membranes, inorganic solid electrolyte film or polymer solid electricity
Solve plasma membrane.
The preparation method of the lithium secondary battery, steps are as follows：
（a）Hydrophobically modified nano-particle is added in organic solvent II, is sufficiently stirred to form gluey slurry；
（b）By step（a）The gluey slurry of preparation is coated on diaphragm both sides, and vacuum drying obtains being coated with nanoparticle coating
Diaphragm；
（c）According to anode pole piece, step（b）The diaphragm for being coated with nanoparticle coating and the cathode pole piece sequence prepared assembles electricity
Core；
（d）Electrolyte is injected into battery core, makes nanoparticle coating swelling to encapsulate battery core after gel electrolyte.
The step（a）Mass fraction of the middle hydrophobically modified nano-particle in organic solvent II is 3-30%, organic solvent
II is one or more of dimethylbenzene, methanol, ethyl alcohol, isopropanol, dioxane or N-Methyl pyrrolidone；Step（b）In
The thickness of gluey slurry coating is 10-100 μm, and vacuum drying temperature is 25-100 DEG C.
The preparation method of the lithium secondary battery, steps are as follows：
（e）Hydrophobically modified nano-particle is added in electrolyte, is sufficiently stirred to form nano-composite gel electrolyte；
（f）By step（e）The nano-composite gel electrolyte double spread of middle preparation is on diaphragm；Obtain coating gel electrolyte
Diaphragm；
（g）According to anode pole piece, step（f）The diaphragm of coating gel electrolyte obtained, cathode pole piece sequence assemble battery core simultaneously
Encapsulation.
The step（e）The mass fraction of hydrophobic nano-particles is 3 ~ 30 %, step in middle nano-composite gel electrolyte
Suddenly（f）The thickness of nano-composite gel electrolyte coating is 5-50 μm.
The beneficial effects of the invention are as follows：Inventive gel electrolyte is the introducing hydrophobically modified nanoparticle in liquid electrolyte
Son forms three dimensional network by hydrophobically modified nano-particle and its surface-modified molecules with the intermolecular hydrogen bond action of electrolyte solvent
Network makes Liquid Electrolyte Gels.The addition of hydrophobically modified nano-particle can effectively improve the lithium ion transference number of electrolyte, and
And the interface impedance gel between electrolyte and lithium metal is reduced, the ionic conductivity and the pure electrolyte of same type of electrolyte are close,
About 10-3S/cm；Compared with the pure electrolyte of same type, there is preferably compatibility between the gel electrolyte and metal lithium electrode and follow
Ring stability；Compared with the pure electrolyte of same type, there is lower interface impedance between the gel electrolyte and metal lithium electrode.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Obtain other attached drawings according to these attached drawings.
Fig. 1 is the process flow chart of the present invention.
Wherein, 1- diaphragms, 2- nano-composite gel electrolytes, 3- positive active materials, 4- negative electrode active materials, 5- anodes
Collector, 6- negative current collectors.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
The every other embodiment that those of ordinary skill in the art are obtained under the premise of not making the creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of lithium secondary battery, structure include：
（1）Anode pole piece comprising plus plate current-collecting body 5 and positive active material 3；
（2）Cathode pole piece comprising negative current collector 6 and negative electrode active material 4；
（3）Diaphragm 1；
（4）Nano-composite gel electrolyte 2 is used to be spaced between diaphragm 1 and anode pole piece and cathode pole piece.
The preparation method of lithium secondary battery is as follows：
（1）Hydrophobic Al2O3The preparation of nano-particle：By Al2O3Nano-particle and silane coupling agent ultrasonic disperse are in ethyl alcohol, and 70
6 h are stirred under the conditions of DEG C, are finally dried in vacuo with ethyl alcohol washed product using centrifugation or filter type separation product.
（2）Anode material nickel cobalt manganese ternary material NCM523 is coated on aluminium foil and prepares anode pole piece；
（3）Lithium metal is combined on copper foil by plating or roll-in mode and prepares cathode pole piece；
（4）By Al2O3Nano-particle is added in electrolyte, is sufficiently stirred and mucilage binding slurry is made.Nano-particle quality in slurry
Score is 15%, and lithium salts used in electrolyte is LiClO4, organic solvent is propene carbonate；
（5）By step（3）For prepared gel electrolyte double spread on porous PE diaphragms, every face coating thickness is 20 μm；
（6）According to anode pole piece, be coated with the diaphragm of gel electrolyte, cathode pole piece sequence assembling battery core and encapsulate.
2 ~ 5 basic step of embodiment is consistent with embodiment 1, except that used positive electrode, nanoparticle subclass
Lithium salts and organic solvent type, diaphragm type, gel electrolyte coating thickness in type, nano-particle mass fraction, electrolyte.Tool
Body see the table below：
1. embodiment of table, 2 ~ 5 parameter
Embodiment 6
The preparation method of lithium secondary battery is as follows：
（1）Hydrophobic SiO2The preparation of nano-particle：By SiO2Nano-particle and silane coupling agent ultrasonic disperse are in ethyl alcohol, and 70
6 h are stirred under the conditions of DEG C, are finally dried in vacuo with ethyl alcohol washed product using centrifugation or filter type separation product.
（2）Anode material nickel cobalt manganese ternary material NCM523 is coated on aluminium foil and prepares anode pole piece；
（3）Lithium metal is combined on copper foil by plating or roll-in mode and prepares cathode pole piece；
（4）By dewatering nano SiO2Particle, which is added in organic solvent to be sufficiently stirred, prepares nano-particle forerunner's slurry, nano-particle
Mass fraction in organic solvent is 6 %, and organic solvent used in forerunner's slurry is ethyl alcohol.
（5）It will（3）On nano-particle forerunner's slurry double spread to PE diaphragms of middle preparation, coating thickness is 30 μm, with
Vacuum drying obtains the diaphragm of coated nanoparticle afterwards；
（6）After appropriate electrolyte being injected according to the sequence assembling battery core of anode pole piece, the diaphragm of coated nanoparticle, cathode pole piece
It encapsulates, lithium salts is LiPF in the electrolyte6, organic solvent is propene carbonate.
7 ~ 10 basic step of embodiment is consistent with embodiment 6, except that used positive electrode, nanoparticle subclass
In type, forerunner's slurry solvent, forerunner's slurry in nano-particle mass fraction, diaphragm type, forerunner's slurry coating thickness, electrolyte
Lithium salts and organic solvent type.Specifically it see the table below：
2. embodiment of table, 7 ~ 9 parameter
Charge-discharge test is carried out to examples detailed above and calculates discharge capacitance, charge-discharge magnification 0.5C.
By the symmetrical non-obstruction batteries of nano-composite gel assembling Li-Li prepared by above-mentioned all embodiments, measure lithium from
The interface impedance of sub- transport number and gel electrolyte confrontation lithium, as a comparison with pure electrolyte.
3 embodiment of table, 1 ~ 10 capacity retention ratio is less than charge and discharge cycles number when 90%, is pair with corresponding pure electrolyte
According to group
Nano-composite gel electrolyte lithium ion transference number in 4 embodiment 1 ~ 10 of table
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of nano-composite gel electrolyte, it is characterised in that：Nano-composite gel electrolyte is by hydrophobically modified nano-particle
It is formed with electrolyte, the mass fraction of hydrophobically modified nano-particle is 3-30% in nano-composite gel electrolyte, for being spaced in
Between battery diaphragm and positive and negative electrode.
2. nano-composite gel electrolyte according to claim 1, it is characterised in that：The hydrophobically modified nano-particle is
Nanometer Al2O3, Nano-meter SiO_22, nano-ZnO, nano SnO2Or nano-TiO2At least one, the hydrophobically modified nano-particle
Size is 5-500 nm.
3. nano-composite gel electrolyte according to claim 1, it is characterised in that：The hydrophobically modified nano-particle profit
Nano-particle is modified with silane coupling agent, the silane coupling agent be hexamethyldisiloxane, dimethyl silicone polymer,
Dimethyl siloxane, octamethylcy-clotetrasiloxane, Trichloromethyl silane, dimethyldichlorosilane, methacryloxypropyl
One or more of trimethoxy silane.
4. nano-composite gel electrolyte according to claim 3, it is characterised in that method of modifying is：By nano-particle with
For silane coupling agent ultrasonic disperse in ethyl alcohol, the mass fraction of nano-particle and silane coupling agent in ethanol is respectively 1 ~ 10%
With 1 ~ 15%, 3 ~ 12 h are stirred under the conditions of 60 ~ 90 DEG C, using centrifugation or filter type separation product, with ethyl alcohol washed product, most
After be dried in vacuo.
5. nano-composite gel electrolyte according to claim 1, it is characterised in that：The electrolyte includes lithium salts and has
Solvent I, the lithium salts are LiClO4、LiPF6, one or more of LiOH, LiTFSI, LiFSI or LiFNFSI；It is described to have
Solvent I is in propene carbonate, ethylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate or methyl propyl carbonate
One or more.
6. the lithium secondary battery prepared using claim 1-5 any one of them nano-composite gel electrolytes, feature are existed
In：The lithium secondary battery includes anode pole piece, cathode pole piece, diaphragm and nano-composite gel electrolyte, described nano combined
Gel electrolyte is made of hydrophobically modified nano-particle and electrolyte, for being spaced between battery diaphragm and positive and negative electrode.
7. the preparation method of the lithium secondary battery described in claim 6, it is characterised in that steps are as follows：
（a）Hydrophobically modified nano-particle is added in organic solvent II, is sufficiently stirred to form gluey slurry；
（b）By step（a）The gluey slurry of preparation is coated on diaphragm both sides, and vacuum drying obtains being coated with nanoparticle coating
Diaphragm；
（c）According to anode pole piece, step（b）The diaphragm for being coated with nanoparticle coating and the cathode pole piece sequence prepared assembles electricity
Core；
（d）Electrolyte is injected into battery core, makes nanoparticle coating swelling to encapsulate battery core after gel electrolyte.
8. the preparation method of lithium secondary battery according to claim 7, it is characterised in that：The step（a）In hydrophobic change
Property mass fraction of the nano-particle in organic solvent II be 3-30%, organic solvent II is dimethylbenzene, methanol, ethyl alcohol, isopropyl
One or more of alcohol, dioxane or N-Methyl pyrrolidone；Step（b）The thickness of middle glue slurry coating is 10-100
μm, vacuum drying temperature is 25-100 DEG C.
9. the preparation method of the lithium secondary battery described in claim 6, it is characterised in that steps are as follows：
（e）Hydrophobically modified nano-particle is added in electrolyte, is sufficiently stirred to form nano-composite gel electrolyte；
（f）By step（e）The nano-composite gel electrolyte double spread of middle preparation is on diaphragm；Obtain coating gel electrolyte
Diaphragm；
（g）According to anode pole piece, step（f）The diaphragm of coating gel electrolyte obtained, cathode pole piece sequence assemble battery core simultaneously
Encapsulation.
10. the preparation method of lithium secondary battery according to claim 9, it is characterised in that：The step（e）Middle nanometer is multiple
The mass fraction for closing hydrophobic nano-particles in gel electrolyte is 3-30 %, step（f）Nano-composite gel electrolyte is coated with
Thickness be 5-50 μm.
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| CN109755656A (en) * | 2019-01-14 | 2019-05-14 | 西北工业大学 | Novel " self-excitation live-in " lithium ion secondary reserve cell of one kind and preparation method thereof |
| CN109888265A (en) * | 2019-01-28 | 2019-06-14 | 南京师范大学 | Silicotitanium interference networks material derived from a kind of hydrogel and its preparation method and application |
| CN110212241A (en) * | 2019-06-12 | 2019-09-06 | 哈尔滨工业大学 | A kind of solid electrolyte membrane and its preparation process and application |
| CN111196888A (en) * | 2020-01-06 | 2020-05-26 | 浙江大学 | Gel polymer electrolyte doped with modified particles and preparation method and application thereof |
| CN111435757A (en) * | 2020-04-02 | 2020-07-21 | 珠海冠宇电池股份有限公司 | Composite polymer electrolyte, preparation method thereof and lithium battery |
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