CN109346767A - A kind of solid polymer electrolyte and its application in lithium metal battery - Google Patents
A kind of solid polymer electrolyte and its application in lithium metal battery Download PDFInfo
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- CN109346767A CN109346767A CN201811292552.9A CN201811292552A CN109346767A CN 109346767 A CN109346767 A CN 109346767A CN 201811292552 A CN201811292552 A CN 201811292552A CN 109346767 A CN109346767 A CN 109346767A
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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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Abstract
A kind of application the present invention relates to solid polymer electrolyte and its in lithium metal battery, it includes polymeric matrix and forms lithium ion conductor in the polymer matrix, and the polymeric matrix is selected from one of polyethers, polycarbonate, polysulfide acid esters or a variety of.Solid electrolyte is obtained and loading lithium ion conductor in particular kind of polymeric matrix, not only have the advantages that excellent dendritic growth inhibits, safety and reliability improves, the advantages of also showing workability, high-flexibility, light weight and high ionic conductivity, low interfacial resistance, suitable for the large-scale application lithium metal battery.
Description
Technical field
The invention belongs to field of lithium, are related to a kind of electrolyte, and in particular to a kind of solid polymer electrolyte and its
Application in lithium metal battery.
Background technique
Lithium ion battery due to having many advantages, such as high-energy density, having extended cycle life is widely used in electronic power supply,
Occupy leading market status.When lithium ion battery by supper-fast charging, discharge or overcharge etc. abuse conditions when, electricity
The high-energy-density density in pond would generally cause energy response, generate huge heat, therefore use the normal of non-aqueous electrolyte
The security risk for advising lithium ion battery is still an important challenge and unsolved obstacle, especially in large scale and high energy
In metric density application system.This is because being grown on lithium anode caused by lithium metal nonuniform deposition after repeated charge
Space between Li dendrite meeting bridged electrodes, leads to internal short-circuit of battery.In volatile electrolyte, by a system of these short circuit generations
Column exothermic reaction may cause overheat and thermal runaway, then further increase internal battery-temperature and pressure, generate catastrophic
Fire or explosion danger；And a possibility that thermal failure it is significant increase with the increase of battery size, be unfavorable for lithium-ion electric
The commercialization of pond group.
In order to inhibit the cause dendritic growth of fever, solid polymer electrolyte is undoubtedly considered as a kind of ideal solution
Certainly scheme.Compared with liquid electrolyte, it has the advantages that excellent dendritic growth inhibits, safety and reliability improves；With
Inorganic ceramic electrolyte phase ratio, makes it at the advantages of also showing workability, high-flexibility, light weight and low interfacial resistance
Suitable for the large-scale application lithium ion battery.Under normal conditions, the polymeric matrix of solid polymer electrolyte is answered
With high dielectric constant, to separate enough lithium salts as lithium ion conductor.
Summary of the invention
One kind is provided the invention aims to overcome the deficiencies in the prior art has room temperature high ionic conductivity and energy
Inhibit the solid polymer electrolyte of lithium dendrite growth.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of solid polymer electrolyte, it include polymerization
The lithium ion conductor of object matrix and formation in the polymer matrix, the polymeric matrix are selected from polyethers, poly- carbonic acid
One of ester, polysulfide acid esters are a variety of.
Optimally, the polymeric matrix carries out polymerization reaction by liquid monomer under the action of catalyst or initiator and obtains
, the liquid monomer is selected from 1,3-dioxolane, tetrahydrofuran, fourth oxygen ring, vinylene carbonate, ethylene carbonate Asia second
Ester, diallyl carbonate, Allyl methyl carbonate, in bis- (2- methacrylic) carbonic esters and vinyl ethylene sulfite
One or more.Specifically, the catalyst be one of strong protonic acid, solid acid, precious metal salt and lewis acid or
It is several；The initiator is selected from one of azo-initiator, organic peroxy class initiator and inorganic peroxy class initiator
Or it is several.
Optimally, it is lithium ion conductor to be dissolved in liquid monomer, then carry out polymerization reaction acquisition；Specifically, lithium
Content of the ion conductor in liquid monomer is 1~2mol/L.
Optimally, the lithium ion conductor is selected from bis trifluoromethyl sulfimide lithium, lithium hexafluoro phosphate, dioxalic acid boric acid
One of lithium, lithium perchlorate, difluorine oxalic acid boracic acid lithium, LiBF4 and trifluoromethyl sulfonic acid lithium or a variety of combinations.
Another object of the present invention is to provide a kind of application of above-mentioned solid polymer electrolyte in lithium metal battery,
The solid polymer electrolyte and anode, cathode are subjected to assembling and form battery, the anode is lithium metal, and the cathode is
Selected from one of LiFePO4, ternary material, nickel ion doped and sulphur carbon material or a variety of.
Optimally, the battery be button cell, the solid polymer electrolyte be assembled with iris-diaphragm, or
Person carries out in-situ polymerization after injecting with liquid.
Optimally, the cathode also includes conductive additive and binder.
Due to the above technical solutions, the present invention has the following advantages over the prior art: solid-state polymerization of the present invention
Object electrolyte obtains solid electrolyte and loading lithium ion conductor in particular kind of polymeric matrix, not only has
The advantages of excellent dendritic growth inhibits, safety and reliability improves, also shows workability, high-flexibility, light weight
The advantages of with high ionic conductivity, low interfacial resistance, suitable for the large-scale application lithium metal battery；It can use original
Position polymerization methods obtain, to realize good contact and the compatibility between solid electrolyte and cathode/anode；It is used for lithium
Metal secondary batteries can greatly improve its cycle performance and security performance.
Detailed description of the invention
Fig. 1 is the scanning electron microscope image of polymer dielectric in-situ polymerization in lithium piece made from embodiment 1；
Fig. 2 is the ionic conductivity figure of solid polyelectrolyte made from embodiment 1；
Fig. 3 is that 1 in-situ polymerization object electrolyte of embodiment assembles lithium Symmetrical cells cyclic polarization curve；
Fig. 4 is that the polymer dielectric of in-situ polymerization prepared by embodiment 1 is applied to the secondary electricity of LiFePO4 // lithium metal
The cycle performance figure in pond；
Fig. 5 is that the polymer dielectric of in-situ polymerization prepared by embodiment 1 is applied to the cycle performance figure of lithium-sulfur cell；
Fig. 6 is the scanning electron microscope image of polymer dielectric in-situ polymerization in lithium piece made from embodiment 14；
Fig. 7 is the ionic conductivity figure of solid polyelectrolyte made from embodiment 14；
Fig. 8 is that 14 in-situ polymerization object electrolyte of embodiment assembles lithium Symmetrical cells cyclic polarization curve；
Fig. 9 is that the polymer dielectric of in-situ polymerization prepared by embodiment 14 is applied to the secondary electricity of LiFePO4 // lithium metal
The cycle performance figure in pond.
Specific embodiment
Solid polymer electrolyte of the present invention, it includes the lithium of polymeric matrix and formation in the polymer matrix
Ion conductor, the polymeric matrix are selected from one of polyethers, polycarbonate, polysulfide acid esters or a variety of.By specific
Lithium ion conductor is loaded in the polymeric matrix of type and obtains solid electrolyte, not only inhibit with excellent dendritic growth,
The advantages of safety and reliability improves, also shows workability, high-flexibility, light weight and high ionic conductivity, lower bound
The advantages of surface resistance, suitable for the large-scale application lithium metal battery；It can use in-situ polymerization mode and obtains, thus
Realize good contact and the compatibility between solid electrolyte and cathode/anode；It is used for lithium metal secondary cell, it can be substantially
Improve its cycle performance and security performance.
Above-mentioned polymeric matrix is usually carried out polymerization reaction acquisition by liquid monomer under the action of catalyst or initiator
(first lithium ion conductor can be dissolved in liquid monomer and form uniform mixed solution, then make mixed solution in catalyst or
Under the action of initiator occur polymerization reaction obtain), the liquid monomer be preferably selected from 1,3-dioxolane, tetrahydrofuran,
Fourth oxygen ring, vinylene carbonate, vinylethylene carbonate, diallyl carbonate, Allyl methyl carbonate, bis- (2- methyl alkene
Propyl) one or more of carbonic ester and vinyl ethylene sulfite.The lithium ion conductor is selected from bis trifluoromethyl
Sulfimide lithium, lithium hexafluoro phosphate, dioxalic acid lithium borate, lithium perchlorate, difluorine oxalic acid boracic acid lithium, LiBF4 and fluoroform
One of base Sulfonic Lithium or a variety of combinations.The catalyst is in strong protonic acid, solid acid, precious metal salt and lewis acid
One or more.The initiator is selected from azo-initiator, organic peroxy class initiator and inorganic peroxy class initiator
One or more of.When lithium ion conductor is dissolved in form uniform mixed solution in liquid monomer when, can to mix
The concentration of lithium ion conductor is 1~2mol/L in solution.
Application of the above-mentioned solid polymer electrolyte in lithium metal battery is by the solid polymer electrolyte and sun
Pole, cathode carry out assembling and form battery, and the anode is lithium metal, and the cathode is selected from LiFePO4, ternary material, nickel manganese
One of sour lithium and sulphur carbon material are a variety of.Above-mentioned battery is usually button cell, the solid polymer electrolyte be with
Iris-diaphragm is assembled, or carries out in-situ polymerization assembling after injecting with liquid.The cathode is usually also comprising conductive addition
Agent and binder；Conductive additive is generally selected from one in carbon black, natural graphite, synthetic graphite, graphene and metallic particles etc.
Kind is a variety of；Binder is then selected from one of Kynoar, polytetrafluoroethylene (PTFE) and carboxymethyl cellulose etc. or a variety of.
Below in conjunction with embodiment, invention is further explained.
Embodiment 1
It is specific as follows the present embodiment provides a kind of solid polymer electrolyte and its application:
In the glove box full of argon gas, bis trifluoromethyl sulfimide lithium (LiTFSI) is dissolved with the concentration of 1mol/L
Homogeneous solution is formed in 1,3-dioxolane (i.e. liquid monomer), and the catalyst lewis acid BF of 1wt% is then added3(its
Mass fraction is using the quality of homogeneous solution as benchmark) it is uniformly mixed and forms polymeric precursor solution, carry out battery pack in situ
Fill to obtain button cell；
Specific assemble method are as follows:
By LiFePO4Material, acetylene black, the PVDF ratio uniform of 8:1:1 in mass ratio are dispersed in N-Methyl pyrrolidone
(NMP) slurry is made in, scratches on aluminium foil, it is the disk of 12mm as battery positive pole piece (pole piece that diameter is cut into after dry
Activity substance content be about 8.0mg/cm2)；Or uniformly, then business sulphur powder and carbon nanotube are ground with mass ratio 6:4
It is encapsulated in vial in 155 DEG C of heating, 24 hours obtained sulphur carbon materials；By sulphur carbon material, the PVDF ratio of 9:1 in mass ratio
It is dispersed in be uniformly dispersed in N-Methyl pyrrolidone (NMP) and slurry is made, be coated on aluminium foil, 24 hours are then heated at 60 DEG C extremely
Drying, as battery positive pole piece, (sulphur load capacity is about 1.2mg/cm2).Using metal lithium sheet as negative pole piece of battery.Assembling button
When formula battery, cathode and diaphragm are put well, precursor solution is injected in button cell, anode is put into, eventually forms button cell,
Specific performance and parameter are shown in Fig. 1 to Fig. 5.Fig. 1 is the scanning of the in-situ polymerization in lithium piece of polymer dielectric made from embodiment 1
Electron microscope image shows have the polymer dielectric of continuous structure attached securely by the in-situ polymerization in assembled battery
Arrive anode lithium on piece, therefore reduce the interface resistance come between self-electrode and electrolyte, be conducive to the electricity of lithium ion battery
Chemical stability.Fig. 2 is the ionic conductivity figure of solid polyelectrolyte made from embodiment 1, is demonstrated by the solid state electrolysis
The high ionic conductivity of matter.Fig. 3 is that 1 in-situ polymerization object electrolyte of embodiment assembles lithium Symmetrical cells cyclic polarization curve, from figure
In as can be seen that the Symmetrical cells can keep the polarization potential of very little for a long time.Fig. 4 is that original position prepared by embodiment 1 is poly-
The polymer dielectric of conjunction is applied to LiFePO4 // lithium metal secondary cell cycle performance figure, and Fig. 5 is prepared by embodiment 1
The polymer dielectric of in-situ polymerization is applied to the cycle performance figure of lithium-sulfur cell, it can be seen that Inventive polymers solid state electrolysis
Matter can maintain LiFePO4 // lithium metal battery and stablizing for lithium-sulfur cell to recycle.
Embodiment 2
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the concentration of bis trifluoromethyl sulfimide lithium is 1.5mol/L.
Embodiment 3
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the concentration of bis trifluoromethyl sulfimide lithium is 2mol/L.
Embodiment 4
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the mass concentration of catalyst is 2%.
Embodiment 5
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the mass concentration of catalyst is 5%.
Embodiment 6
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the catalyst used is strong protonic acid fluosulfonic acid.
Embodiment 7
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the catalyst used is precious metal salt AgSbF6。
Embodiment 8
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the lithium ion conductor used is lithium perchlorate.
Embodiment 9
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the lithium ion conductor used is dioxalic acid lithium borate.
Embodiment 10
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the lithium ion conductor used is difluorine oxalic acid boracic acid lithium.
Embodiment 11
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the lithium ion conductor used is trifluoromethyl sulfonic acid lithium.
Embodiment 12
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: liquid monomer uses tetrahydrofuran.
Embodiment 13
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: liquid monomer uses fourth oxygen ring.
Embodiment 14
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: liquid monomer uses diallyl carbonate, and initiator is that azodiisobutyronitrile (be shown in by the specific performance and parameter of final battery
Fig. 6 to Fig. 9).Fig. 6 is the scanning electron microscope diagram of the in-situ polymerization in lithium piece of polymer dielectric made from embodiment 14
Picture shows that the in-situ polymerization that again may be by assembled battery with the polymer dielectric is firmly adhered to anode lithium piece
On.Fig. 7 is the ionic conductivity figure of solid polyelectrolyte made from embodiment 14, be demonstrated by the solid electrolyte it is high from
Electron conductivity.Fig. 8 is that 14 in-situ polymerization object electrolyte of embodiment assembles lithium Symmetrical cells cyclic polarization curve, can therefrom be seen
Out, which generates voltage fluctuation in lithium deposition/stripping process almost without with time/period, this is attributed to solid
Stable interface between state polymeric dielectric and lithium metal surface.Moreover, not having after the long-term polarization at 100 hours yet
There is observable short circuit.Fig. 9 is that the polymer dielectric of in-situ polymerization prepared by embodiment 14 is applied to ferric phosphate
Lithium // lithium metal secondary cell cycle performance figure, it can be seen that Inventive polymers solid electrolyte can maintain ferric phosphate
Lithium // lithium metal battery circulation steady in a long-term.
Embodiment 15
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the mass concentration of initiator is 2%.
Embodiment 16
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: the mass concentration of catalyst is 5%.
Embodiment 17
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: liquid monomer uses vinyl ethylene sulfite.
Embodiment 18
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: liquid monomer uses bis- (2- methacrylic) carbonic esters.
Embodiment 19
The present embodiment provides a kind of solid polymer electrolyte and its application, it and it is almost the same in embodiment 1, it is different
: liquid monomer uses Allyl methyl carbonate.
LiFePO4 of the table 1 based on 1~13 solid polymer electrolyte of embodiment // lithium metal battery chemical property is surveyed
Try performance table
Lithium-sulfur cell electrochemical property test performance table of the table 2 based on 1~13 solid polymer electrolyte of embodiment
| Initial capacity | Circulating ring number | Recycle conservation rate | |
| Embodiment 1 | 850 | 100 | 75% |
| Embodiment 2 | 860 | 100 | 72% |
| Embodiment 3 | 865 | 100 | 73% |
| Embodiment 4 | 800 | 100 | 70% |
| Embodiment 5 | 730 | 100 | 65% |
| Embodiment 6 | 500 | 100 | 50% |
| Embodiment 7 | 600 | 100 | 61% |
| Embodiment 8 | 810 | 100 | 70% |
| Embodiment 9 | 450 | 100 | 40% |
| Embodiment 10 | 400 | 100 | 38% |
| Embodiment 11 | 830 | 100 | 68% |
| Embodiment 12 | 730 | 100 | 67% |
| Embodiment 13 | 640 | 100 | 65% |
LiFePO4 of the table 3 based on 14~19 solid polymer electrolyte of embodiment // lithium metal battery chemical property is surveyed
Try performance table
| Initial capacity | Circulating ring number | Recycle conservation rate | |
| Embodiment 14 | 149 | 50 | 100% |
| Embodiment 15 | 142 | 50 | 93% |
| Embodiment 16 | 139 | 50 | 88% |
| Embodiment 17 | 110 | 50 | 85% |
| Embodiment 18 | 127 | 50 | 87% |
| Embodiment 19 | 129 | 50 | 77% |
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of solid polymer electrolyte, it includes the lithium ion of polymeric matrix and formation in the polymer matrix
Conductor, it is characterised in that: the polymeric matrix is selected from one of polyethers, polycarbonate, polysulfide acid esters or a variety of.
2. solid polymer electrolyte according to claim 1, it is characterised in that: the polymeric matrix is by liquid monomer
Polymerization reaction acquisition is carried out under the action of catalyst or initiator, the liquid monomer is selected from 1,3-dioxolane, tetrahydro
Furans, fourth oxygen ring, vinylene carbonate, vinylethylene carbonate, diallyl carbonate, Allyl methyl carbonate, bis- (2- first
Base allyl) one or more of carbonic ester and vinyl ethylene sulfite.
3. solid polymer electrolyte according to claim 1, it is characterised in that: it is that lithium ion conductor is dissolved in liquid
In state monomer, then carry out polymerization reaction acquisition.
4. solid polymer electrolyte according to claim 1, it is characterised in that: the lithium ion conductor is selected from double three
Methyl fluoride sulfimide lithium, lithium hexafluoro phosphate, dioxalic acid lithium borate, lithium perchlorate, difluorine oxalic acid boracic acid lithium, LiBF4 and
One of trifluoromethyl sulfonic acid lithium or a variety of combinations.
5. solid polymer electrolyte according to claim 2, it is characterised in that: the catalyst is strong protonic acid, admittedly
One or more of body acid, precious metal salt and lewis acid.
6. solid polymer electrolyte according to claim 2, it is characterised in that: the initiator is to draw selected from azo
Send out one or more of agent, organic peroxy class initiator and inorganic peroxy class initiator.
7. solid polymer electrolyte according to claim 3, it is characterised in that: the content of the lithium ion conductor be 1 ~
2mol/L。
8. application of any solid polymer electrolyte in lithium metal battery in claim 1 to 7, it is characterised in that:
The solid polymer electrolyte and anode, cathode are subjected to assembling and form battery, the anode is lithium metal, and the cathode is
Selected from one of LiFePO4, ternary material, nickel ion doped and sulphur carbon material or a variety of.
9. application of the solid polymer electrolyte in lithium metal battery according to claim 8, it is characterised in that: the electricity
Pond is button cell, and the solid polymer electrolyte is to be assembled with iris-diaphragm, or carry out after being injected with liquid former
Position polymerization.
10. application of the solid polymer electrolyte in lithium metal battery according to claim 8, it is characterised in that: described
Cathode also includes conductive additive and binder.
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