CN107732293B - The preparation method of class sandwich structure solid polymer electrolyte membrane and its application in solid lithium ion battery - Google Patents

The preparation method of class sandwich structure solid polymer electrolyte membrane and its application in solid lithium ion battery Download PDF

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Publication number
CN107732293B
CN107732293B CN201710881439.3A CN201710881439A CN107732293B CN 107732293 B CN107732293 B CN 107732293B CN 201710881439 A CN201710881439 A CN 201710881439A CN 107732293 B CN107732293 B CN 107732293B
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polymer electrolyte
solution
sandwich structure
electrolyte membrane
solid polymer
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CN107732293A (en
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岳红云
王秋娴
李静娴
董红玉
尹艳红
杨书廷
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Xinxiang Battery Research Institute Co Ltd
Henan Normal University
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Xinxiang Battery Research Institute Co Ltd
Henan Normal University
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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
    • 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
    • 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
    • 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
    • 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
    • H01M2300/0088—Composites
    • H01M2300/0091—Composites in the form of mixtures
    • 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
    • H01M2300/0088—Composites
    • H01M2300/0094—Composites in the form of layered products, e.g. coatings
    • 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 the preparation method of a type sandwich structure solid polymer electrolyte membrane and its applications in solid lithium ion battery, belong to solid lithium ion battery technical field.Technical solution of the present invention main points are as follows: take mass ratio to be dissolved in acetonitrile for the polymer and alkali metal salt of 2 ~ 6:1, be uniformly mixed to obtain solution A；It takes half solution A and plasticizer is added thereto, be thoroughly mixed and uniformly obtain solution B；Solution A and solution B is respectively coated on support membrane two sides, is subsequently placed in vacuum oven dry 12 ~ class sandwich structure solid polymer electrolyte membrane is made for 24 hours.The invention also discloses the preparation methods for the solid lithium ion battery for using such sandwich structure solid polymer electrolyte membrane.Class sandwich structure solid polymer electrolyte membrane ionic conductivity, preferable mechanical strength and low interface impedance with higher prepared by the present invention and good interface stability, effectively improve the cyclical stability of solid lithium ion battery.

Description

The preparation method of class sandwich structure solid polymer electrolyte membrane and its in solid-state lithium Application in ion battery
Technical field
The invention belongs to solid lithium ion battery technical fields, and in particular to a type sandwich structure solid polymer electricity The preparation method for solving plasma membrane and its application in solid lithium ion battery.
Background technique
In recent years, lithium ion battery is because many merits such as its energy density is high, have extended cycle life, self-discharge rate is low are by people It is widely used in the especially various portable electronic products of numerous areas.With the development and progress of society, lithium-ion electric Pond also becomes one of pure electric vehicle power vehicle and the best candidate in hybrid electric vehicle power source.However, current commercial lithium Ion battery mostly uses easily leakage, volatile, explosive organic electrolyte, greatly reduces the security performance of lithium ion battery And energy density.Therefore replace traditional liquid electrolyte that can efficiently solve the above problem using solid electrolyte.Solid-state Electrolyte is divided into inorganic solid electrolyte and organic solid-state polymer dielectric.Inorganic solid electrolyte intensity is good, but without bullet Property, not easy to be processed, this will lead to the big problem of interface impedance between electrolyte and electrode, it is difficult to carry out commercial applications.And have Machine solid polymer electrolyte not only has certain conductivity, but also the characteristic with high molecular polymer, is lithium ion Battery provides available material to directions such as solid state, safe, ultrathins.Meanwhile organic polyelectrolyte also can be significantly Promote the development of wearable electronic product.
Currently, the main problem that solid polymer electrolyte faces is that conductivity at room temperature is low, interface impedance is big, mechanical Intensity is not high.Polycarbonates have good conductivity at room temperature, interface compatibility and chemical stability, still Mechanical performance is bad.After metal salt is dissolved in polymer, then with support membrane carry out compound, obtained solid polymer electrolyte membrane It is provided simultaneously with good ionic conductivity and mechanical property, is greatly reduced interface impedance, this is mentioned for the application of solid state battery A new power is supplied.
Summary of the invention
The main object of the present invention be solve low conductivity, high interface impedance that existing solid polymer electrolyte faces and The problems such as poor mechanical performance and provide a type sandwich structure solid polymer electrolyte membrane preparation method and its Application in solid lithium ion battery.
The present invention adopts the following technical scheme that achieve the above object, class sandwich structure solid polymer electrolyte membrane, It is characterized in that wherein including polymerization in solution A as being respectively coated made from solution A and solution B in support membrane two sides Object and alkali metal salt, include polymer, alkali metal salt and plasticizer in solution B, and the support membrane is polypropylene screen or nonwoven Measuring fiber film, the polymer are polyethylene glycol oxide (PEO), polypropylene carbonate (PPC), polyethylencarbonate (PEC), poly- carbon Sour vinylene (PVC), polyacrylonitrile (PAN), Kynoar-hexafluoropropene (PVDF-HFP) or polymethyl methacrylate One of (PMMA) or a variety of, the alkali metal salt is LiN (SO2CF3)2(LiTFSI), LiN (SO2F)2(LiFSI), LiClO4、LiB(C2O4)2(LiBOB) or LiBC2O4F2One of (LiDFOB) or a variety of, the plasticizer is succinonitrile (SN), one of diethyl phthalate (DEP), ethylene carbonate (EC) or polyethylene glycol dimethyl ether (PEGDME) or more Kind.
The preparation method of class sandwich structure solid polymer electrolyte membrane, it is characterised in that specific steps are as follows:
(1) it takes mass ratio to be dissolved in acetonitrile for the polymer and alkali metal salt of 2 ~ 6:1, is uniformly mixed to obtain solution A；
(2) it takes half solution A and plasticizer is added thereto, be thoroughly mixed and uniformly obtain solution B；
(3) solution A and solution B is respectively coated on support membrane two sides, it is subsequently placed in vacuum oven dry 12 ~ it makes for 24 hours Obtain class sandwich structure solid polymer electrolyte membrane.
A kind of preparation method of the solid lithium ion battery using class sandwich structure solid polymer electrolyte membrane, it is special Sign is specific steps are as follows: is close to the one side of prepared class sandwich structure solid polymer electrolyte membrane coating solution B It is placed on class sandwich structure solid polymer electrolyte membrane coating solution A on positive plate, then by negative electrode tab, in argon gas gloves Solid lithium ion battery is assembled into case.
Further preferably, the positive electrode active materials in the positive plate are nickle cobalt lithium manganate, cobalt acid lithium, LiFePO4 or manganese Sour lithium.
Further preferably, the negative electrode material in the negative electrode tab is lithium titanate, graphite, lithium metal or lithium indium alloy.
In the preparation method of solid lithium ion battery provided by the invention, solid polymer electrolyte membrane uses class Sanming City Structure is controlled, the solid polymer electrolyte membrane of coating solution A one side can increase electrode and solid polymer electrolyte well Between contact, to improve the cyclical stability of solid state battery.The solid polymer electrolyte membrane of coating solution B one side contains There is plasticizer, the contact internal resistance between positive-active layer and solid polymer electrolyte can be reduced, improves lithium ion conductivity. Support membrane can increase the mechanical performance of solid polymer electrolyte.
Detailed description of the invention
Fig. 1 is the impedance diagram of solid lithium ion battery at room temperature made from embodiment 1 and comparative example 1；
Fig. 2 is the cycle performance figure of solid lithium ion battery made from embodiment 1 and comparative example 1.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair Bright range.
Embodiment 1
The preparation of positive plate:
According to the mass percent of 80:10:10 by iron phosphate serving as positive active material, conductive agent acetylene black and binder PPC is added in appropriate anhydrous acetonitrile, is uniformly mixed and is configured to slurry and is coated on aluminium foil, then puts it into 40 DEG C Dry 30min in baking oven is then dry in 80 DEG C of vacuum tanks to obtain iron phosphate lithium positive pole piece for 24 hours.
The preparation of class sandwich structure solid polymer electrolyte membrane:
It takes PPC 1g and alkali metal salt LiTFSI 0.5g to be dissolved in appropriate acetonitrile, is uniformly mixed to obtain solution A；It takes Simultaneously 0.2g plasticizer SN is added in half solution A thereto, is thoroughly mixed and uniformly obtains solution B；On polypropylene screen two sides point Other coating solution A and solution B obtain similar sandwich structure solid polymer electrolyte after being put into vacuum oven dry 12h Plasma membrane.
The preparation of solid lithium ion battery:
Prepared class sandwich structure solid polymer electrolyte membrane coating solution B is tightly attached to LiFePO4 on one side On positive plate, then metal lithium sheet is placed on class sandwich structure solid polymer electrolyte membrane coating solution A, in argon gas gloves Solid lithium ion battery is assembled into case.
Fig. 1 gives the impedance diagram of solid lithium ion battery made from the present embodiment at room temperature, and test is using occasion China CHI760B type electrochemical workstation.
Fig. 2 gives the cycle performance figure of solid lithium ion battery made from the present embodiment.As seen from the figure, pass through this method The solid lithium ion battery of preparation class sandwich structure solid polymer electrolyte membrane, shows excellent chemical property.
Embodiment 2
The preparation of positive plate:
According to the mass percent of 70:10:20 by positive electrode active materials nickel cobalt manganese, conductive agent acetylene black and binder PEO It is added in appropriate anhydrous acetonitrile, is uniformly mixed and is configured to slurry and is coated on aluminium foil, then put it into 40 DEG C of bakings Dry 30min in case is then dry in 80 DEG C of vacuum tanks to obtain nickle cobalt lithium manganate positive plate for 24 hours.
The preparation of class sandwich structure solid polymer electrolyte membrane:
It takes PEO 1g and alkali metal salt LiTFSI 0.17g to be dissolved in appropriate acetonitrile, is uniformly mixed to obtain solution A；It takes Simultaneously 0.6g plasticizer SN is added in half solution A thereto, is thoroughly mixed and uniformly obtains solution B；In non-woven fabrics fiber film two Solution A and solution B is respectively coated in face, obtains similar sandwich structure solid polymer after being put into vacuum oven dry 12h Dielectric film.
The preparation of solid lithium ion battery:
Prepared class sandwich structure solid polymer electrolyte membrane coating solution B is tightly attached to nickel cobalt mangaic acid on one side On lithium positive plate, then metal lithium sheet is placed on class sandwich structure solid polymer electrolyte membrane coating solution A, in argon gas hand Solid lithium ion battery is assembled into casing.
Comparative example 1
The comparative example difference from Example 1 is: it is poly- to be coated with solution B formation monolayer solid on polypropylene screen two sides Polymer electrolyte membrane replaces class sandwich structure solid polymer electrolyte membrane.
Fig. 1 gives the impedance diagram of solid lithium ion battery made from this comparative example at room temperature, and test is using occasion China CHI760B type electrochemical workstation.
Fig. 2 gives the cycle performance figure of solid lithium ion battery made from this comparative example.
Class sandwich structure solid electrolyte membrane prepared by the present invention can contact well with positive plate, greatly reduce Interface impedance, applies and shows excellent chemical property in solid lithium ion battery.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within In the scope of protection of the invention.

Claims (3)

1. a kind of preparation method of the solid lithium ion battery using class sandwich structure solid polymer electrolyte membrane, feature It is specific steps are as follows: by being tightly attached on positive plate on one side for class sandwich structure solid polymer electrolyte membrane coating solution B, For reducing the contact internal resistance between positive-active layer and solid polymer electrolyte to improve lithium ion conductivity, then by cathode Piece is placed on class sandwich structure solid polymer electrolyte membrane coating solution A, for increasing electrode and solid polymer electrolyte Contact between matter is assembled into solid lithium ion battery in argon gas glove box to improve the cyclical stability of solid state battery；
The class sandwich structure solid polymer electrolyte membrane is by the way that solution A and solution B is respectively coated in support membrane two sides It is obtained, wherein include polymer and alkali metal salt in solution A, includes polymer, alkali metal salt and plasticising in solution B Agent, the support membrane are polypropylene screen or non-woven fabrics fiber film, and the polymer is polyethylene glycol oxide, polypropylene carbonate, gathers In ethylene carbonate, polymerized thylene carbonate vinyl acetate, polyacrylonitrile, Kynoar-hexafluoropropene or polymethyl methacrylate One or more, the alkali metal salt is LiN (SO2CF3)2、LiN(SO2F)2、LiClO4、LiB(C2O4)2Or LiBC2O4F2In One or more, the plasticizer is in succinonitrile, diethyl phthalate, ethylene carbonate or polyethylene glycol dimethyl ether It is one or more；
The specific preparation process of the class sandwich structure solid polymer electrolyte membrane are as follows:
(1) it takes mass ratio to be dissolved in acetonitrile for the polymer and alkali metal salt of 2 ~ 6:1, is uniformly mixed to obtain solution A；
(2) it takes half solution A and plasticizer is added thereto, be thoroughly mixed and uniformly obtain solution B；
(3) solution A and solution B is respectively coated on support membrane two sides, is subsequently placed in vacuum oven dry 12 ~ class is made for 24 hours Sandwich structure solid polymer electrolyte membrane.
2. the solid lithium ion battery using class sandwich structure solid polymer electrolyte membrane according to claim 1 Preparation method, it is characterised in that: positive electrode active materials in the positive plate are nickle cobalt lithium manganate, cobalt acid lithium, LiFePO4 Or LiMn2O4.
3. the solid lithium ion battery using class sandwich structure solid polymer electrolyte membrane according to claim 1 Preparation method, it is characterised in that: negative electrode material in the negative electrode tab is lithium titanate, graphite, lithium metal or lithium indium alloy.
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CN111180788B (en) * 2020-03-02 2022-03-22 珠海冠宇电池股份有限公司 All-solid-state electrolyte, preparation method thereof and lithium ion battery
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