CN110233286A - A kind of compound organic solid electrolyte of in-situ polymerization and the preparation method and application thereof - Google Patents
A kind of compound organic solid electrolyte of in-situ polymerization and the preparation method and application thereof Download PDFInfo
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- CN110233286A CN110233286A CN201910223172.8A CN201910223172A CN110233286A CN 110233286 A CN110233286 A CN 110233286A CN 201910223172 A CN201910223172 A CN 201910223172A CN 110233286 A CN110233286 A CN 110233286A
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- 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
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Abstract
The invention discloses compound organic solid electrolytes of a kind of in-situ polymerization and the preparation method and application thereof, the raw material composition of the solid electrolyte includes polymerisable monomer, photoinitiator, inorganic mineral clay and lithium salts, after polymerisable monomer and inorganic mineral clay are uniformly dispersed, coated on pole piece, using ultraviolet light-initiated method, monomer polymerized in situ, is made solid electrolyte, and method is simple and efficient.The present invention is compound by inorganic mineral clay and polymer, and the branched structure of polymer reduces crystallinity, the conduction conducive to lithium ion in amorphous region；Inorganic mineral clay used has hollow nano tubular structure, it is possible to provide lithium ion transport channel effectively improves the ionic conductivity of electrolyte.Moreover, the compound polymer dielectric of inorganic mineral clay has higher electrochemical stability window and better thermal stability.
Description
Technical field
The present invention relates to all-solid lithium-ion battery technical field, specially a kind of compound organic solid state electrolysis of in-situ polymerization
Matter and the preparation method and application thereof.
Background technique
With the quickening of modernization, occur in global range the increasingly deficient energy crisis of traditional fossil energy,
The ecological problems such as serious environmental pollution and Global Greenhouse Effect.In face of the environment and resource problem increasingly highlighted, when business
It is suddenly accelerated development clean energy resource, establishes efficient, cleaning, economic, safety energy system, reduce orthodox car industry and industry
The sustainable development of new energy is realized in dependence to fossil energy.With the lithium that can be quickly charged and discharged with the advantages such as environmental-friendly
Ion battery becomes the hot spot of new energy field.
Most of electrolyte used by commercial li-ion battery is liquid electrolyte at present.This battery is faced with two
Very severe problem: first, in battery charge and discharge process, organic solvent can form solid electrolyte membrane in anode, make electrode
Polarization, cell performance decay；Second, the organic solvent as used in electrolyte is hidden in the presence of safety such as leakage, burning, explosions
Suffer from, safety problem causes anxiety.Liquid electrolyte is replaced using solid electrolyte, can effectively improve the security performance of lithium ion battery
And cycle life.
The compatibility of organic solid-state electrolyte and electrode is good, and interface impedance is small；With good mechanical property, can effectively press down
The generation of cathode of lithium dendrite processed；And preparation method is simple, has good filming performance, and it can be by reducing dielectric film
Thickness promotes the energy density of lithium battery, is closest to commercially produce a kind of solid electrolyte of application.But it is lower from
Electron conductivity significantly limits the application of organic solid-state electrolyte.Studies have shown that by inorganic particulate it is compound with polymer be to mention
Nano silica, nano aluminium oxide, Ke Yiti is added in one of effective measures of high ionic conductivity such as in polyethylene glycol oxide
The ionic conductivity of high polyethylene glycol oxide.
Summary of the invention
It is an object of the invention to solve the problems, such as that current organic solid-state electrolyte ion conductivity is lower, and disclose one
Kind compound organic solid electrolyte of in-situ polymerization and the preparation method and application thereof.
The purpose of the present invention is achieved through the following technical solutions.
A kind of compound organic solid electrolyte of in-situ polymerization, raw material composition include polymerisable monomer, photoinitiator, inorganic mine
Object clay and lithium salts.
Further, the polymerisable monomer is polyethylene glycol acrylate monomethyl ether or polyethylene glycol methacrylate-styrene polymer
Monomethyl ether；The inorganic mineral clay is galapectite.
Further, the lithium salts is lithium perchlorate, lithium hexafluoro phosphate or double trifluoromethanesulfonimide lithiums；The light draws
Hair agent is -1 phenylacetone of benzoin dimethylether or 2- hydroxy-2-methyl.
Further, the mass ratio of polymerisable monomer, photoinitiator, inorganic mineral clay and lithium salts is 1:0.01:
(0.04~0.12): (0.10~0.30).
The present invention also provides the preparation method of the compound organic solid electrolyte of the in-situ polymerization, which includes
Following steps:
(1) photoinitiator and lithium salts are added in polymerisable monomer, stirring and dissolving obtains transparent mixing liquid；
(2) inorganic mineral clay is added in the transparent mixing liquid of step (1), is stirred, is uniformly dispersed
Slurry；
(3) slurry in step (2) is coated on pole piece, free radical polymerization is carried out under the illumination of ultraviolet lamp, is obtained
Compound organic solid electrolyte.
Further, step (1)-(3) are to complete in an inert gas atmosphere.
Further, stirring is and to stir 3-4h under the conditions of being protected from light in the step (1)；It is stirred in the step (2)
Mixing the time is 5-6h.
Further, pole piece is stainless steel substrates in the step (3).
Further, ultraviolet lamp power is 80W~120W in step (3), and light application time is 1h~2h.
Compound organic solid electrolyte can be used for all-solid lithium-ion battery, and ionic conductivity be up to 7.1 ×
10-5S cm-1。
Compared with the existing technology, the present invention disperses inorganic mineral clay in polymerisable monomer, by finely dispersed slurry
Material be coated in pole piece on, using ultraviolet light-initiated monomer in situ polymerization, preparation method is simple and efficient, and prepare electrolyte with
Pole piece interfacial contact is good.After monomer polymerization formed main chain be carbon-carbon bond, the branched polymer that side chain is poly glycol monomethyl ether,
Branched structure largely reduces the crystallinity of polymer, increases amorphous region, is conducive to polymer segment transmission
Lithium ion.Inorganic mineral clay galapectite used is hollow nano tubular structure, and this architecture provides lithium ion transport channels, is increased
More delivering paths of lithium ion, can cooperate with branched polymer to improve ionic conductivity, so as to improve all-solid lithium-ion battery
Capacity and cycle life.
Present invention feature and advantage outstanding is:
1. the present invention, by branched polymer and inorganic mineral clay In-situ reaction, inorganic mineral clay used is hollow nanometer
Tubular structure, it is possible to provide lithium ion transport channel；And branched polymer has more compared to traditional crystallinity polyethylene glycol oxide
The amorphous region of large scale, the conduction conducive to lithium ion in amorphous region.The two synergistic effect, can be improved solid electrolyte from
Electron conductivity is up to 7.1 × 10 using the ionic conductivity of the battery of compound organic solid electrolyte in the present invention-5S cm-1And electrochemical stability window reaches 5.22V.
2. present invention in-situ polymerization directly on pole piece prepares compound organic solid electrolyte, gained electrolyte and pole piece
Interfacial contact is good；The compound polymer dielectric of inorganic mineral clay has better thermal stability, and thermal decomposition temperature is high
Up to 341 DEG C.
3. the present invention prepares compound organic solid electrolyte using the method for ultraviolet light-initiated in-situ polymerization, raw material is mixed
After uniformly, the electrolyte can be obtained using UV illumination, for traditional solution casting method, this method environmental protection
Efficiently, device therefor is at low cost and simple to operation.
Specific embodiment
Specific implementation of the invention is described further below in conjunction with specific embodiment, but implementation of the invention is not limited to
This.
Embodiment 1
The preparation of the compound organic solid electrolyte of in-situ polymerization, comprising the following steps:
Step 1, in argon gas glove box, by polyethylene glycol acrylate monomethyl ether, benzoin dimethylether and double fluoroforms
Alkane sulfimide lithium is added in vial by quality 1g, 0.01g, 0.30g, is protected from light stirring 3 hours, so that solid dissolves, is obtained
To transparency liquid；
0.04g galapectite is added in argon gas glove box in step 2 in the transparency liquid described in step 1, stirring 6 is small
When, prepare finely dispersed slurry；
Slurry made from step 2 is coated on stainless steel substrates by step 3 in argon gas glove box, ultraviolet in 120W
Illumination 1h under lamp carries out Raolical polymerizable, obtains compound organic solid electrolyte.
Compound organic solid electrolyte obtained is assembled into button cell in argon gas glove box, is handed at 30 DEG C
Flow impedance test, measuring ionic conductivity is 7.1 × 10-5S cm-1。
Linear sweep voltammetry test is carried out to compound organic solid electrolyte of preparation, electrochemical stability window can reach
To 5.22V.Thermogravimetric analysis test is carried out to compound organic solid electrolyte of preparation, thermal decomposition temperature is up to 341 DEG C.
Embodiment 2
The preparation of the compound organic solid electrolyte of in-situ polymerization, comprising the following steps:
Step 1, in argon gas glove box, by polyethylene glycol acrylate monomethyl ether, -1 phenyl third of 2- hydroxy-2-methyl
Ketone and lithium hexafluoro phosphate are added in vial by quality 1g, 0.015g, 0.20g, stirring 4 hours are protected from light, so that solid is molten
Solution, obtains transparency liquid；
0.05g galapectite is added in argon gas glove box in step 2 in the transparency liquid described in step 1, stirring 5 is small
When, prepare finely dispersed slurry；
Slurry made from step 2 is coated on stainless steel substrates by step 3 in argon gas glove box, ultraviolet in 100W
Illumination 2h under lamp carries out Raolical polymerizable, obtains compound organic solid electrolyte.
Compound organic solid electrolyte obtained is assembled into button cell in argon gas glove box, is handed at 30 DEG C
Flow impedance test, measuring ionic conductivity is 6.3 × 10-5S cm-1。
Linear sweep voltammetry test is carried out to compound organic solid electrolyte of preparation, electrochemical stability window can reach
To 5.18V.Thermogravimetric analysis test is carried out to compound organic solid electrolyte of preparation, thermal decomposition temperature is 336 DEG C.
Embodiment 3
The preparation of the compound organic solid electrolyte of in-situ polymerization, comprising the following steps:
Step 1, in argon gas glove box, by polyethylene glycol methacrylate-styrene polymer monomethyl ether, -1 benzene of 2- hydroxy-2-methyl
Benzylacetone and lithium perchlorate are added in vial by quality 1g, 0.013g, 0.10g, stirring 3.5 hours are protected from light, so that solid
Dissolution, obtains transparency liquid；
0.07g galapectite is added in argon gas glove box in step 2 in the transparency liquid described in step 1, stirring 5 is small
When, prepare finely dispersed slurry；
Slurry made from step 2 is coated on stainless steel substrates by step 3 in argon gas glove box, ultraviolet in 120W
Illumination 1.5h under lamp carries out Raolical polymerizable, obtains compound organic solid electrolyte.
Compound organic solid electrolyte obtained is assembled into button cell in argon gas glove box, is handed at 30 DEG C
Flow impedance test, measuring ionic conductivity is 5.2 × 10-5S cm-1。
Linear sweep voltammetry test is carried out to compound organic solid electrolyte of preparation, electrochemical stability window can reach
To 5.21V.Thermogravimetric analysis test is carried out to compound organic solid electrolyte of preparation, thermal decomposition temperature is 338 DEG C.
Embodiment 4
The preparation of the compound organic solid electrolyte of in-situ polymerization, comprising the following steps:
Step 1, in argon gas glove box, by polyethylene glycol methacrylate-styrene polymer monomethyl ether, benzoin dimethylether and high chlorine
Sour lithium is added in vial by quality 1g, 0.02g, 0.15g, is protected from light stirring 4 hours, so that solid dissolves, obtains transparent liquid
Body；
0.12g galapectite, stirring 5.5 is added in argon gas glove box in step 2 in the transparency liquid described in step 1
Hour, prepare finely dispersed slurry；
Slurry made from step 2 is coated on stainless steel substrates, in argon gas glove box in 80W ultraviolet lamp by step 3
Lower illumination 1h carries out Raolical polymerizable, obtains compound organic solid electrolyte.
Compound organic solid electrolyte obtained is assembled into button cell in argon gas glove box, is handed at 30 DEG C
Flow impedance test, measuring ionic conductivity is 5.7 × 10-5S cm-1。
Linear sweep voltammetry test is carried out to compound organic solid electrolyte of preparation, electrochemical stability window can reach
To 5.16V.Thermogravimetric analysis test is carried out to compound organic solid electrolyte of preparation, thermal decomposition temperature is 335 DEG C.
Embodiment 5
The preparation of the compound organic solid electrolyte of in-situ polymerization, comprising the following steps:
Step 1, in argon gas glove box, by polyethylene glycol acrylate monomethyl ether, -1 phenyl third of 2- hydroxy-2-methyl
Ketone and double trifluoromethanesulfonimide lithiums are added in vial by quality 1g, 0.01g, 0.23g, are protected from light stirring 3 hours, so that
Solid dissolution, obtains transparency liquid；
0.11g galapectite is added in argon gas glove box in step 2 in the transparency liquid described in step 1, stirring 5 is small
When, prepare finely dispersed slurry；
Slurry made from step 2 is coated on stainless steel substrates by step 3 in argon gas glove box, ultraviolet in 100W
Illumination 1h under lamp carries out Raolical polymerizable, obtains compound organic solid electrolyte.
Compound organic solid electrolyte obtained is assembled into button cell in argon gas glove box, is handed at 30 DEG C
Flow impedance test, measuring ionic conductivity is 5.9 × 10-5S cm-1。
Linear sweep voltammetry test is carried out to compound organic solid electrolyte of preparation, electrochemical stability window can reach
To 5.17V.Thermogravimetric analysis test is carried out to compound organic solid electrolyte of preparation, thermal decomposition temperature is 337 DEG C.
Embodiment 6
The preparation of the compound organic solid electrolyte of in-situ polymerization, comprising the following steps:
Step 1, in argon gas glove box, by polyethylene glycol methacrylate-styrene polymer monomethyl ether, -1 benzene of 2- hydroxy-2-methyl
Benzylacetone and double trifluoromethanesulfonimide lithiums are added in vial by quality 1g, 0.012g, 0.11g, and it is small to be protected from light stirring 4
When, so that solid dissolves, obtain transparency liquid；
0.12g galapectite, stirring 5.5 is added in argon gas glove box in step 2 in the transparency liquid described in step 1
Hour, prepare finely dispersed slurry；
Slurry made from step 2 is coated on stainless steel substrates by step 3 in argon gas glove box, ultraviolet in 120W
Illumination 1.3h under lamp carries out Raolical polymerizable, obtains compound organic solid electrolyte.
Compound organic solid electrolyte obtained is assembled into button cell in argon gas glove box, is handed at 30 DEG C
Flow impedance test, measuring ionic conductivity is 6.7 × 10-5S cm-1。
Linear sweep voltammetry test is carried out to compound organic solid electrolyte of preparation, electrochemical stability window can reach
To 5.20V.Thermogravimetric analysis test is carried out to compound organic solid electrolyte of preparation, thermal decomposition temperature is up to 338 DEG C.
Comparative example 1
Comparative example 1 is organic solid-state electrolyte, not compound with inorganic mineral clay, the substantially same embodiment of the preparation process
1, it is a difference in that omission step 2, that is, is added without galapectite, the ionic conductivity of gained solid electrolyte is lower, and only 1.1
×10-5S cm-1, and its electrochemical stability window only has 4.9V, thermal decomposition temperature is 320 DEG C.
The foregoing is only a preferred embodiment of the present invention, not does restriction in any form to the present invention.It is all
Any equivalent variation that those skilled in the art makes above-described embodiment using technical solution of the present invention is modified or is drilled
Become etc., all of which are still within the scope of the technical scheme of the invention.
Claims (10)
1. a kind of compound organic solid electrolyte of in-situ polymerization, which is characterized in that it includes polymerisable monomer that raw material, which forms, light-initiated
Agent, inorganic mineral clay and lithium salts.
2. the compound organic solid electrolyte of in-situ polymerization according to claim 1, which is characterized in that the monomer is poly- second two
Alcohol acrylate monomethyl ether or polyethylene glycol methacrylate-styrene polymer monomethyl ether；The inorganic mineral clay is galapectite.
3. the compound organic solid electrolyte of in-situ polymerization according to claim 1, which is characterized in that the photoinitiator is peace
The fragrant double methyl ethers of breath or 2- hydroxy-2-methyl -1- phenylacetone；The lithium salts is lithium perchlorate, lithium hexafluoro phosphate or double fluoroforms
Alkane sulfimide lithium.
4. the compound organic solid electrolyte of in-situ polymerization according to claim 1, which is characterized in that example meter in mass ratio, it can
Polymerized monomer, photoinitiator, inorganic mineral clay and lithium salts ratio be 1:(0.01 ~ 0.02): (0.04 ~ 0.12): (0.10 ~
0.30).
5. the method for preparing any one of the claim 1-4 compound organic solid electrolyte of the in-situ polymerization, which is characterized in that packet
Include following steps:
(1) photoinitiator and lithium salts are added in polymerisable monomer, stirring and dissolving obtains transparent mixing liquid；
(2) inorganic mineral clay is added in the transparent mixing liquid of step (1), is stirred, obtain finely dispersed slurry
Material；
(3) slurry in step (2) is coated on pole piece, free radical polymerization is carried out under the illumination of ultraviolet lamp, obtained described
Compound organic solid electrolyte.
6. the preparation method of compound organic solid electrolyte according to claim 5, which is characterized in that step (1)-(3) are equal
It is to complete in an inert gas atmosphere.
7. the preparation method of compound organic solid electrolyte according to claim 5, which is characterized in that ultraviolet in step (3)
Lamp power is 80W ~ 120W, and light application time is 1h ~ 2h.
8. the preparation method of compound organic solid electrolyte according to claim 5, which is characterized in that in the step (1)
Stirring is that 3-4h is stirred under the conditions of being protected from light；Mixing time is 5-6h in the step (2).
9. the preparation method of compound organic solid electrolyte according to claim 5, which is characterized in that in the step (3)
Pole piece is stainless steel substrates.
10. application of any one of the claim 1-4 compound organic solid electrolyte in all-solid lithium-ion battery.
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| CN111900468A (en) * | 2020-08-11 | 2020-11-06 | 珠海冠宇电池股份有限公司 | Solid electrolyte, preparation method thereof and lithium ion battery |
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| CN114512714A (en) * | 2022-01-20 | 2022-05-17 | 贵阳学院 | Composite polymer electrolyte material, preparation method thereof and lithium ion battery |
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| CN114512714A (en) * | 2022-01-20 | 2022-05-17 | 贵阳学院 | Composite polymer electrolyte material, preparation method thereof and lithium ion battery |
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