CN107195963A - A kind of polymer dielectric of high conductivity and preparation method thereof - Google Patents
A kind of polymer dielectric of high conductivity and preparation method thereof Download PDFInfo
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- CN107195963A CN107195963A CN201710249328.0A CN201710249328A CN107195963A CN 107195963 A CN107195963 A CN 107195963A CN 201710249328 A CN201710249328 A CN 201710249328A CN 107195963 A CN107195963 A CN 107195963A
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- polymer
- lithium
- high conductivity
- polymer dielectric
- makrolon
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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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- 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
- H01M2300/0082—Organic polymers
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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
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of polymer dielectric of high conductivity and preparation method thereof, polymer dielectric of the invention is mixed by the makrolon for being dissolved with lithium salts with substrate polymer;Wherein, the makrolon of lithium salts is dissolved with as matrix, and it is conductive component;Substrate polymer is supporter.The polymer dielectric of the present invention prepares simple, room-temperature conductivity height.
Description
Technical field
The present invention relates to chemical production field, and in particular to a kind of polymer dielectric of high conductivity and its preparation side
Method.
Background technology
At present, traditional fossil energy exhausted energy crisis and increasingly serious environment increasingly are faced with global range
Problem.Therefore, develop new energy, set up efficiently, cleaning, economic, safety energy system it is extremely urgent.Because lithium battery has
Energy density is high, have extended cycle life, memory-less effect, can fast charging and discharging the advantages of, set as irreplaceable excellent energy storage
It is standby.Lithium battery is very fast by having developed since Sony companies formally commercialization from early 1990s, it has also become at present in hand
Most common main flow energy storage device on the small size digital electronic product such as machine, notebook computer and digital camera.However, traditional lithium electricity
Pond use liquid electrolyte, have the shortcomings that it is volatile, inflammable, explosive, with major safety risks.With lithium ion battery
To developing rapidly in terms of large-sized power power supply application field such as pure electric automobile, Aero-Space and large-scale energy storage, battery
Capacity and energy density constantly increase, and its current ratio and power density are also improved constantly, using be more and more extensively so that
The safety problem of lithium battery is set to protrude increasingly.
On the other hand, polymer electrolyte battery have have a safety feature, energy density is high, operating temperature it is interval it is wide, follow
The advantages of ring long lifespan and have been widely recognized, be the study hotspot of field of lithium ion battery.
Up to the present, the conventional polymer dielectric of lithium ion battery mainly includes:Kynoar-hexafluoropropene,
Polyacrylonitrile, polyacrylamide, polymethyl methacrylate, polyoxyethylene, polyoxypropylene etc..But these polymer have one
Fixed shortcoming, although for example polyoxyethylene, polyoxypropylene can be used as full solid state polymer electrolyte, however, it is low from
Electron conductivity limits their application.It can be said that currently without each side such as electrical conductivity, electrochemical stability and interface stabilitys
The gratifying polymer dielectric of face performance.
The content of the invention
To solve above-mentioned problems of the prior art, the present invention provide a kind of high conductivity polymer dielectric and
Its preparation method, the polymer dielectric that provides of the present invention is solid-state, and its conductance is high safe while.
The polymer dielectric of the high conductivity of the present invention, the electrolyte is gathered by the makrolon for being dissolved with lithium salts with substrate
Compound is mixed, wherein, the makrolon of lithium salts is dissolved with as matrix, and it is conductive component;Substrate polymer is support
Body.
The polymer dielectric of high conductivity as described above, the lithium salts is dispersed in the polycarbonate matrix, institute
The mass ratio stated substrate polymer and be dissolved with the makrolon of lithium salts is 1:9-9:1, the content of lithium salts in the makrolon
For.The mass ratio particularly preferred 1 of the substrate polymer and the makrolon for being dissolved with lithium salts:9-1:1;It is described
The mass ratio particularly preferred 1 of substrate polymer and the makrolon for being dissolved with lithium salts:9-1:5, the substrate polymer is with dissolving
The mass ratio for having the makrolon of lithium salts is more highly preferred to 1:9-1:4.
According to the polymer dielectric of high conductivity as described above, the makrolon is poly- ethylene carbonate, poly- carbon
One or more in acid propylene ester or polymerized thylene carbonate vinyl acetate.
According to the polymer dielectric of high conductivity as described above, the lithium salts is lithium perchlorate, lithium hexafluoro phosphate, two
Lithium bis (oxalate) borate, hexafluoroarsenate lithium, LiBF4, trifluoromethyl sulfonic acid lithium, bis trifluoromethyl sulfimide lithium or double fluorine sulphurs
One or more in imide li.
According to the polymer dielectric of high conductivity as described above, the substrate polymer is poly-methyl methacrylate
Ester, polyethylene glycol oxide, Kynoar, poly- (biasfluoroethylene-hexafluoropropylene), one kind in polyacrylonitrile, polyvinyl alcohol or several
Kind.
According to the polymer dielectric of high conductivity as described above, the polymer dielectric is also containing 1-50wt%'s
Inorganic filler and/or fast-ionic conductor.
According to the polymer dielectric of high conductivity as described above, the inorganic filler be silica, titanium dioxide,
It is one or more of in alundum (Al2O3), zirconium oxide, nickel oxide, silicon nitride, magnesium hydroxide, diatomite, montmorillonite and kaolin;Institute
Fast-ionic conductor is stated for Li7La3Zr2O12、Li10GeP2S12、Li3OCl0.5Br0.5、Li3xLa(2/3)-xTiO3、Li5La3Ta2O12、
Li5La3Nb2O12、Li5 .5La3Nb1 .75In0.25O12、Li3N-LiCl、Li3N-LiBr、Li3N-LiI、Li14Zn( GeO4 )4、
LiZr2( PO4 )3、Li3OCl, LiPON and Li2One or more in S-MaSb, wherein, 0 .04<x<0 .14, M=Al, Si
Or P, a and b value are respectively 1-3.
According to the method for preparing polymer electrolytes of high conductivity as described above, it comprises the steps:
(1)First makrolon is dissolved in solvent, poly- carbon ester solution is obtained;
(2)Lithium salts is added in poly- carbon ester solution, stirring is to being completely dissolved;
(3)Substrate polymer is added into solution, stirring obtains polymer dielectric to being completely dissolved after drying.
According to preparation method as described above, it is in step 3) in, by inorganic filler and/or fast-ionic conductor and substrate
Polymer adds solution simultaneously, the solution for mixing homogeneous.
According to preparation method as described above, the solvent be acetonitrile, dimethyl sulfoxide (DMSO), sulfolane, dimethyl sulfite,
Sulfurous acid diethyl ester, acetone, tetrahydrofuran, chloroform, ethyl acetate, N,N-dimethylformamide, N, N- dimethylacetamides
One or more in amine, 1-METHYLPYRROLIDONE.
Fig. 1 is the internal structure schematic diagram of the solid polymer electrolyte of the present invention.As shown in figure 1, the polymerization of the present invention
Thing electrolyte, its entirety is solid-state, and makrolon is matrix, and substrate polymer is supporter, and substrate polymer is dispersed in poly-
In carbonic ester, lithium ion and the anion also random dispersion that lithium salts is constituted with lithium ion, lithium ion carries out conductive.
The polymer dielectric preparation method of the present invention is simple, and room-temperature conductivity is high, electrochemistry and interface stability are good.
Brief description of the drawings
Fig. 1 is the internal structure schematic diagram of the solid polymer electrolyte of the present invention.
Fig. 2 is the oxidation Decomposition potential diagram of obtained solid polymer electrolyte membrane in embodiment 1.
Fig. 3 is the testing impedance figure of obtained solid polymer electrolyte membrane in embodiment 1.
Embodiment
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
The poly- ethylene carbonates of 2.7g and 100g 1-METHYLPYRROLIDONEs are added into 250 ml reagent bottles 6 h acquisitions are stirred at room temperature
Even solution, 1.8g bis trifluoromethyl sulfimide lithiums are added among above-mentioned solution, 6 h are stirred at normal temperatures, treat completely molten
0.5g Kynoar is added after solution, stirring obtains uniform mixed solution, and the mixed solution is injected into polytetrafluoroethylene (PTFE)
(PTFE)Film forming is dried in mould, vacuum drying obtains solid polymer electrolyte membrane.
Embodiment 2
The poly- ethylene carbonates of 0. 5 g and 100g dimethyl sulfites are added into 250 ml reagent bottles 6 h acquisitions are stirred at room temperature
Even solution, the double fluorine sulfimide lithiums of 4.5g are added among above-mentioned solution, 6 h are stirred at normal temperatures, are added until completely dissolved
Enter 1.25g to gather(Biasfluoroethylene-hexafluoropropylene), stirring obtains uniform mixed solution, by mixed solution injection polytetrafluoroethyl-ne
Alkene(PTFE)Film forming is dried in mould, vacuum drying obtains solid polymer electrolyte membrane.
Embodiment 3
3g polypropylene carbonates and 100 g acetonitriles are added into 100 ml reagent bottles 6 h acquisition homogeneous solutions are stirred at room temperature, by 3g
Lithium perchlorate is added among above-mentioned solution, and 6 h are stirred at normal temperatures, and 6g polyvinyl alcohol is added until completely dissolved, is stirred
To uniform mixed solution, the mixed solution is injected into polytetrafluoroethylene (PTFE)(PTFE)Film forming is dried in mould, vacuum drying is produced
To solid polymer electrolyte membrane.
Embodiment 4
6 h are stirred at room temperature in 0.9 g polymerized thylene carbonates vinyl acetate and 100g tetrahydrofurans 250 ml reagent bottles of addition and obtain uniform molten
Liquid, 3.6g trifluoromethyl sulfonic acid lithiums are added among above-mentioned solution, and 6 h are stirred at normal temperatures, are added until completely dissolved
After 0.56 polyacrylonitrile, fully dissolving, 2.5g nanometer silicon dioxide particles are added, stirring obtains uniform mixed solution, by this
Mixed solution injects polytetrafluoroethylene (PTFE)(PTFE)Film forming is dried in mould, vacuum drying obtains solid polymer electrolyte membrane.
Embodiment 5
6 h are stirred at room temperature in 0.9 g polymerized thylene carbonates vinyl acetate and 100g chloroforms 250 ml reagent bottles of addition and obtain uniform molten
Liquid, 2.1g LiBF4s are added among above-mentioned solution, and 6 h are stirred at normal temperatures, and the poly- first of 27g is added until completely dissolved
After base methyl acrylate, fully dissolving, 3g Li are added5La3Ta2O12, stirring obtains uniform mixed solution, by the mixed solution
Inject polytetrafluoroethylene (PTFE)(PTFE)Film forming is dried in mould, vacuum drying obtains solid polymer electrolyte membrane.
Embodiment 6
0.3g polypropylene carbonates and 100 g acetonitriles are added into 100 ml reagent bottles 6 h acquisition homogeneous solutions are stirred at room temperature, will
0.3g lithium perchlorates are added among above-mentioned solution, and 6 h are stirred at normal temperatures, and 4.2g polyethylene is added until completely dissolved
Alcohol, stirring obtains uniform mixed solution, and the mixed solution is injected into polytetrafluoroethylene (PTFE)(PTFE)Film forming, vacuum are dried in mould
Drying to obtain solid polymer electrolyte membrane.
Embodiment 7
3.6g polypropylene carbonates and 100 g acetonitriles are added into 100 ml reagent bottles 6 h acquisition homogeneous solutions are stirred at room temperature, will
0.9g lithium perchlorates are added among above-mentioned solution, and 6 h are stirred at normal temperatures, and 13.5g polyethylene is added until completely dissolved
Alcohol, stirring obtains uniform mixed solution, and the mixed solution is injected into polytetrafluoroethylene (PTFE)(PTFE)Film forming, vacuum are dried in mould
Drying to obtain solid polymer electrolyte membrane.
Comparative example 1
By polyethylene glycol oxide 10g, lithium perchlorate 2g, after solvent acetonitrile 200g is well mixed, it is poured into mould and dries film forming, very
Empty drying to obtain solid polymer dielectric film.
Ionic conductivity, ionic conductance are determined to obtained solid polymer dielectric film in embodiment 1-7 and comparative example 1
Rate test specific method be:Using electrochemical workstation, the friendship of battery is blocked by determining stainless steel/electrolyte/stainless steel
Flow impedance obtains polymer dielectric ionic conductivity to calculate.Specifically testing procedure is:, will in the glove box full of argon gas
Dielectric film is clipped between two stainless steel substrates, is assembled into obstruction battery, starts software, and setting frequency range is 1 Hz ~ 10
MHz, amplitude is 10 mV, can set the temperature parameter of needs to test the AC impedance of present battery.Experimental result obtains one
Straight line, the intersection point numerical value that straight line intersects with real axis is the bulk resistance of electrolyte, is designated as Rm.The ionic conductivity of electrolyte
Calculation formula:.In formula:σ is ionic conductivity, and L is the thickness of electrolyte;S is that barrier film connects with electrode
Tactile area;Rm is bulk resistance.
Table 1
As shown in Table 1, its room-temperature conductivity of polymer dielectric produced by the present invention is especially excellent.In addition, Fig. 1 is embodiment 1
In obtained solid polymer electrolyte membrane oxidation Decomposition potential diagram.Fig. 2 is obtained solid polymer electrolyte in embodiment 1
The testing impedance figure of plasma membrane.As shown in Figure 1, oxidation Decomposition current potential>4.5V, obtained solid polymer electrolyte membrane electrochemistry is steady
It is qualitative good.As shown in Figure 2, impedance increase is not obvious after stabilization, and obtained solid polymer electrolyte membrane shows interface stability
It is good.
Claims (10)
1. a kind of polymer dielectric of high conductivity, it is characterised in that the electrolyte by be dissolved with the makrolon of lithium salts with
Substrate polymer is mixed;Wherein, the makrolon of lithium salts is dissolved with as matrix, and it is conductive component;Substrate polymer
For supporter.
2. the polymer dielectric of high conductivity according to claim 1, it is characterised in that the lithium salts is dispersed in described
In polycarbonate matrix, the mass ratio of makrolon of the substrate polymer with being dissolved with lithium salts is 1:9-9:1, the poly- carbon
The content of lithium salts is 40-90wt% in acid esters.
3. the polymer dielectric of high conductivity according to claim 2, it is characterised in that the substrate polymer with it is molten
The mass ratio that solution has the makrolon of lithium salts is 1:9-1:1.
4. the polymer dielectric of high conductivity according to claim 1 or 2, it is characterised in that the makrolon is
One or more in poly- ethylene carbonate, polypropylene carbonate or polymerized thylene carbonate vinyl acetate;The lithium salts is lithium perchlorate, six
Lithium fluophosphate, dioxalic acid lithium borate, hexafluoroarsenate lithium, LiBF4, trifluoromethyl sulfonic acid lithium, bis trifluoromethyl sulfimide
One or more in lithium or double fluorine sulfimide lithiums.
5. the polymer dielectric of high conductivity according to claim 1 or 2, it is characterised in that the substrate polymer
For polymethyl methacrylate, polyethylene glycol oxide, Kynoar, poly- (biasfluoroethylene-hexafluoropropylene), polyacrylonitrile, poly- second
One or more in enol.
6. the polymer dielectric of high conductivity according to claim 1, it is characterised in that the polymer dielectric is also
Inorganic filler and/or fast-ionic conductor containing 1~50wt%.
7. the polymer dielectric of high conductivity according to claim 6, it is characterised in that the inorganic filler is dioxy
SiClx, titanium dioxide, alundum (Al2O3), zirconium oxide, nickel oxide, silicon nitride, magnesium hydroxide, diatomite, montmorillonite and kaolin
Middle one or more;The fast-ionic conductor is Li7La3Zr2O12、Li10GeP2S12、Li3OCl0.5Br0.5、、Li5La3Ta2O12、Li5La3Nb2O12、Li5 .5La3Nb1 .75In0.25O12、Li3N-LiCl、
、Li3N-LiI、Li14Zn( GeO4 )4、LiZr2( PO4 )3、Li3OCl, LiPON and Li2One or more in S-MaSb, its
In, 0 .04<x<0 .14, M=Al, Si or P, a and b value are respectively 1-3.
8. the method for preparing polymer electrolytes of the high conductivity according to claim 1-7, it is characterised in that including under
State step:
(1)First makrolon is dissolved in solvent, poly- carbon ester solution is obtained;
(2)Lithium salts is added in poly- carbon ester solution, stirring is to being completely dissolved;
(3)Substrate polymer is added into solution, stirring obtains polymer dielectric to being completely dissolved after drying.
9. preparation method according to claim 8, it is characterised in that in step 3) in, by inorganic filler and/or it is fast from
Sub- conductor adds solution simultaneously with substrate polymer, the solution for mixing homogeneous.
10. preparation method according to claim 8 or claim 9, it is characterised in that the solvent is acetonitrile, dimethyl sulfoxide (DMSO), ring
Fourth sulfone, dimethyl sulfite, sulfurous acid diethyl ester, acetone, tetrahydrofuran, chloroform, ethyl acetate, N, N- dimethyl formyls
One or more in amine, DMAC N,N' dimethyl acetamide, 1-METHYLPYRROLIDONE.
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Cited By (9)
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CN108598566A (en) * | 2018-04-23 | 2018-09-28 | 浙江大学山东工业技术研究院 | A kind of modified polymer electrolyte film and preparation method thereof and a kind of modified gel polymer electrolyte |
CN108711609A (en) * | 2018-05-15 | 2018-10-26 | 清陶(昆山)新能源材料研究院有限公司 | A kind of lithium an- ode process of surface treatment and its application |
CN108832176A (en) * | 2018-06-01 | 2018-11-16 | 西北工业大学 | A kind of cellulose/polycarbonate solid polymer dielectric and preparation method |
CN108832177A (en) * | 2018-06-01 | 2018-11-16 | 西北工业大学 | A kind of POSS compound cellulose/polycarbonate solid polymer dielectric and preparation method |
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CN108711609B (en) * | 2018-05-15 | 2021-09-17 | 苏州清陶新能源科技有限公司 | Lithium metal negative electrode surface treatment process and application thereof |
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CN108832177A (en) * | 2018-06-01 | 2018-11-16 | 西北工业大学 | A kind of POSS compound cellulose/polycarbonate solid polymer dielectric and preparation method |
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CN108987815A (en) * | 2018-08-28 | 2018-12-11 | 长沙矿冶研究院有限责任公司 | A kind of obstruction battery assembly method improving obstruction cell interface contact |
CN109449483A (en) * | 2018-11-05 | 2019-03-08 | 浙江众泰汽车制造有限公司 | A kind of compound for lithium-sulfur cell electrolyte, lithium-sulfur cell electrolyte and preparation method thereof, solid-state lithium-sulfur cell |
CN109755643B (en) * | 2018-12-28 | 2020-11-10 | 浙江大学 | Oxygen-enriched polymer electrolyte and preparation method and application thereof |
CN109755643A (en) * | 2018-12-28 | 2019-05-14 | 浙江大学 | A kind of oxygen-enriched polymer dielectric and its preparation method and application |
CN109755638B (en) * | 2018-12-29 | 2021-05-11 | 浙江南都电源动力股份有限公司 | Composite electrolyte membrane, preparation method and application thereof |
CN109755638A (en) * | 2018-12-29 | 2019-05-14 | 浙江南都电源动力股份有限公司 | The preparation method and applications of composite electrolyte membrane, composite electrolyte membrane |
CN114424379A (en) * | 2019-07-19 | 2022-04-29 | 道达尔能源公司 | Solid polymer electrolyte comprising polycarbonate olefin ester |
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