CN106876784A - A kind of PEO bases solid polymer electrolyte membrane and preparation method thereof - Google Patents
A kind of PEO bases solid polymer electrolyte membrane and preparation method thereof Download PDFInfo
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- CN106876784A CN106876784A CN201710003124.9A CN201710003124A CN106876784A CN 106876784 A CN106876784 A CN 106876784A CN 201710003124 A CN201710003124 A CN 201710003124A CN 106876784 A CN106876784 A CN 106876784A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
It is to be related to a kind of PEO bases solid polymer electrolyte membrane and preparation method thereof specifically the invention belongs to technical field of chemical power.It includes polymeric matrix and alkali metal salt, and the EO/Li mass ratioes of polymeric matrix and alkali metal salt are 5~30：1；Polymer is the copolymer of polyethylene glycol oxide (PEO) and polymethyl methacrylate (PMMA), and the molecular weight of PEO is that 100000~1000000, PMMA molecular weight is 25000~100000；Alkali metal salt is LiClO4、LiPF6、LiBF4、LiTFSI、LiAsF6、Li B(C2O4)2(Li BOB)、Li SO2CF3(Li Tf) more than one.
Description
Technical field：
It is to be related to a kind of PEO bases solid polymer electrolyte membrane specifically the invention belongs to technical field of chemical power
And preparation method thereof.
Background technology：
All solid lithium secondary battery, i.e. battery each component, including both positive and negative polarity, electrolyte are all using the lithium two of solid-state material
Primary cell.The polymer dielectric of solid-state is used because of it, instead of traditional liquid electrolyte, to make the secondary electricity of polymer Li-ion
Pond have the advantages that can thin type, arbitrary areaization and arbitrary shape, will not also produce in the safety such as leakage and combustion explosion
Problem.
Polyethylene glycol oxide (PEO) main chain contains strong electron donating group, and Mi Yang functional groups are in the network constituted with alkali metal (MX)
In zoarium system PEO as ion conducting matrix Li+ as charge carriers component, the slaine under the ether oxygen atom effect of strand
Electric charge carrier is dissociated into, is migrated in polymeric media by the short range sub-chain motion ion of polymer and is shown ion and lead
Electrical property.PEO good lithium ion conduction ability is because it has crystal structure and undefined structure concurrently.Therefore, as PEO is non-
The increase electrical conductivity of crystalline region is continuously increased.Cause electrical conductivity at room temperature relatively low however, PEO is easily crystallized, significantly limit PEO
The application of base polymer electrolyte.
In recent years, because PMMA undefined structures can reach 96% while having good chemical stability and machinery
Performance, therefore PEO and PMMA blendings are prepared composite polymer electrolyte membrane by many people.However, only both is combined,
The thermal property and electric property of film are poor.
Liquid Crystalline Ionomer (LCI) is the Ionomer with liquid crystal polymer feature.This kind of ionomer combine from
The double-deck performance of polymers and liquid crystal, by introducing ion, the diatropism of liquid crystal polymer is improved using ion interphase interaction
Energy.And montmorillonite (MMT) can play the effect of plasticizer in the base, the crystallinity of PEO can be to a certain extent reduced.
The two Dominant Facies is combined using Liquid Crystalline Ionomer/montmorillonite hybrid material, it is significant for improving electrical conductivity.
The content of the invention：
The present invention is exactly regarding to the issue above, there is provided a kind of preparation method is simple, it is electric at room temperature to improve lithium battery
Conductance, the PEO bases solid polymer electrolyte membrane and its system of extensive industrialization that is easy to operate, being suitable for solid lithium battery
Preparation Method.
To achieve these goals, the present invention is adopted the following technical scheme that, including polymeric matrix and alkali metal salt, polymerization
The O/Li mass ratioes of thing matrix and alkali metal salt are 5~30：1；
Polymer is the copolymer of polyethylene glycol oxide (PEO) and polymethyl methacrylate (PMMA), and the molecular weight of PEO is
100000~1000000, PMMA molecular weight are 25000~100000；
Alkali metal salt is LiClO4、LiPF6、LiBF4、LiTFSI、LiAsF6、Li B(C2O4)2(Li BOB)、Li SO2CF3
(Li Tf) more than one.
Specific preparation process is,
1st, the preparation of blend solution
By PEO with 0.5~1.5:The solid-liquid ratio of 20~100g/ml is dissolved in dichloromethane, and is statically placed in iodine flask
Middle 12h, then by PMMA with 0.05~1：The solid-liquid ratio of 10~50g/ml is dissolved in dichloromethane, is added to after stirring and dissolving is complete molten
Solve in the dichloromethane solution of PEO, be stirred well to dissolving completely, the mass ratio of PEO and PMMA is 0.5~1.5 in mixed liquor：
0~1, then again to lithium perchlorate is added in mixed liquor, it is stirred at room temperature to dissolving fully, PEO is with the mass ratio of lithium perchlorate
0.5~1.5：0.01-1, is put into rotor in iodine flask, sealing, at 25 DEG C, with 700rmp rotating speed magnetic agitations 90min；
2nd, the preparation of blend film
Weigh LCI/MMT hybrid material 1-METHYLPYRROLIDONEs and dissolving is shaken in test tube, the solid-liquid ratio of the two is
0.001~0.5:1~20g/ml, to being added in the solution of LCI/MMT, PEO/PMMA solution blendings stirring obtained in step 1 is equal
It is even, solid-liquid ratio 1~20:30~150g/ml, using automatic knifing machine knifing on a glass, blade thickness is 0.5mm, will be made
2h is dried at 50 DEG C of the film air dry oven for obtaining, matrix, sealing preserve are peeled off with blade；
3rd, cell package
Blend film obtained in step 2 is encapsulated into stainless steel battery, the composition material material of battery is stainless steel, sealed
Ultrasonic oil removal is carried out using ultrasonic cleaner before dress, encapsulation order is：Negative pole+shell fragment+pad+dielectric film+pad+pad
Piece+positive pole → small-sized hydraulic button cell packaging machine hydraulic pressure encapsulation.
The structure of LCI is in LCI/MMT hybrid materials in step 2,
In film slicing processes, whole dielectric film is cut into slices using manual button cell slicer, need to be beaten using A4
Printing paper doubling coats dielectric film, and correspondence dielectric film uniform parts are cut after pressing, same with what dielectric film together cut
Sample shape A4 paper will sandwich hermetic electrolyte plasma membrane, be taken out during using tweezers, dielectric film is pressed from both sides from the scraps of paper, using calibrator to electricity
Solution plasma membrane thickness measuring.With the electrolyte membrane samples after scraps of paper sealing preserve thickness measuring after record data.Sealing preserve is standby.
Beneficial effects of the present invention：
The present invention prepares into full solid state polymer electrolyte material, polymer electrolytic of the invention using simple knifing method
Material without organic liquid electrolytes in the absence of electrolyte leakage problem, non-combustible, the shape and thickness of film are controllable, film into
Mould is good, homogeneous.And compared with traditional PEO base polymer electrolytes, electrical conductivity can reach 4.00 × 10-3S cm-
1, while mechanical performance is excellent.
Brief description of the drawings：
Fig. 1 is the AC impedance Nyquist curve maps of polymer dielectric film.
Fig. 2 is the scanning electron microscopic picture of electrical conductivity highest example.
Specific embodiment：
Comparative example
PEO (0.7g) is dissolved in dichloromethane (40ml) and is statically placed in 12h in iodine flask, then take PMMA (0.3g) and be dissolved in
Dichloromethane (10ml), added to after stirring and dissolving is complete dissolving PEO dichloromethane solution in.It is sufficiently stirred for, is suitably heated to
Dissolving is complete, adds lithium perchlorate (0.1g) and is stirred at room temperature to dissolving fully.Above-mentioned mixed solution is added into dissolving PEO-
In the iodine flask of the dichloromethane of PMMA, rotor is put into, sealed, with 700rmp rotating speed magnetic agitations 90min at 25 DEG C.
Using automatic knifing machine at the uniform velocity knifing on smooth glass plate, scraper is highly set to 0.5mm to the solution that will be prepared, will
The glass plate for having scraped film is placed in 50 DEG C of drying 24h in air dry oven.Peeled off with blade.Sealing preserve.
It is encapsulated into stainless steel battery, the composition material material of battery is stainless steel, and ultrasonic wave is used before encapsulation
Washer carries out ultrasonic oil removal.Encapsulation order be：Negative pole+shell fragment+pad+dielectric film+pad+pad+positive pole → small-sized
Hydraulic pressure button cell packaging machine hydraulic pressure is encapsulated.
All-solid-state composite polymer electrolyte film is placed between two stainless steel electrodes of known area, obstruction electricity is made
Pond.Using EIS AC impedence method test ion electrical conductivity, with electrochemical analyser, its AC impedance is surveyed, survey ac impedance spectroscopy
Frequency sweeping ranges between 1Hz-100kHz, ac-excited signal be 5mV.To ensure the height of electrode surface in test process
The planarization of degree, while also requiring to ensure electrolyte and electrode comprehensive engagement, exists, therefore use stainless without bubble between the two
Steel button cell box produces test battery, reuses supporting battery case connection test circuit.
The treatment of gained ac impedance spectroscopy carries software and carries out Equivalent Circuit Fitting analysis using instrument, for resulting
Polymer dielectric, its ac impedance spectroscopy equivalent circuit diagram can obtain the resistance of PEO/PMMA films as simulated by equivalent circuit
Rb, then calculates the ionic conductivity of PEO/PMMA films according to following formula
σ=L/ (RbS)
Wherein, the thickness (cm) of L-polymer dielectric film material；
S-participate in the area (cm of the polymer dielectric film material of reaction2)；
The bulk resistance (Ω) of Rb-polymer dielectric.
The blending electrolyte membrane samples of pulverization process are tested using differential scanning analyzer.Programming rate is 20
DEG C/min, -50-300 DEG C of temperature elevating range.The thickness of obtained film is 0.036mm.
Example 1
PEO (0.7g) is dissolved in dichloromethane (40ml) and is statically placed in 12h in iodine flask, then take PMMA (0.3g) and be dissolved in
Dichloromethane (10ml), added to after stirring and dissolving is complete dissolving PEO dichloromethane solution in.It is sufficiently stirred for, is heated to dissolving
Completely, lithium perchlorate (0.1g) is added to be stirred at room temperature to dissolving fully.To being put into rotor in iodine flask, seal, at 25 DEG C with
700rmp rotating speed magnetic agitations 90min.
Weigh LCI/MMT hybrid materials (0.004g) 2ml 1-METHYLPYRROLIDONEs and dissolving is shaken in test tube, will
The solution of LCI/MMT adds PEO/PMMA solution blendings to stir, and using automatic knifing machine knifing on a glass, scraper is thick
Degree is set to 0.5mm.Automatic scraping homogeneous film, after obtained film is dried into 2h using 50 DEG C of air dry oven, is shelled with blade
From matrix.45 DEG C of vacuum drying 12h thoroughly remove solvent again.
Using automatic knifing machine at the uniform velocity knifing on smooth glass plate, scraper is highly set to 0.5mm to the solution that will be prepared, will
The glass plate for having scraped film is placed in 50 DEG C of drying 24h in air dry oven.Peeled off with blade.Sealing preserve.
It is encapsulated into stainless steel battery, the composition material material of battery is stainless steel, and ultrasonic wave is used before encapsulation
Washer carries out ultrasonic oil removal.Encapsulation order be：Negative pole+shell fragment+pad+dielectric film+pad+pad+positive pole → small-sized
Hydraulic pressure button cell packaging machine hydraulic pressure is encapsulated.
The thickness of obtained film is 0.039mm.
Example 2
With not existing together for LCI/MMT hybrid materials addition is 0.007g for embodiment 1.
The thickness of obtained film is 0.033mm.
Example 3：
With not existing together for LCI/MMT hybrid materials addition is 0.01g for embodiment 1.
The thickness of obtained film is 0.031mm.
Fig. 1 is the AC impedance Nyquist curves of polymer dielectric film, it can be seen that the low frequency of example 3 (SPEs-M3)
Area is minimum with transverse axis intersection point, Rb=24.62 Ω, conductivityσ=4.00 × 10-3.Fig. 2 is the scanning electron microscopic picture of example 3, can
It is close to find out hybrid material particle size in film, it is uniformly dispersed,
Example 4：
With not existing together for LCI/MMT hybrid materials addition is 0.014g for embodiment 1.
The thickness of obtained film is 0.030mm.
Example 5：
With not existing together for LCI/MMT hybrid materials addition is 0.017g for embodiment 1.
The thickness of obtained film is 0.037mm.
Example 6：
With not existing together for LCI/MMT hybrid materials addition is 0.020g for embodiment 1.
The thickness of obtained film is 0.038mm.
Table 1 is the thermodynamic parameter of polymer dielectric film
Claims (3)
1. a kind of PEO bases solid polymer electrolyte membrane, it is characterised in that including polymeric matrix and alkali metal salt, polymer
The EO/Li mass ratioes of matrix and alkali metal salt are 5~30：1；
Polymer is the copolymer of polyethylene glycol oxide and polymethyl methacrylate, the molecular weight of PEO for 100000~
1000000, PMMA molecular weight are 25000~100000；
Alkali metal salt is LiClO4、LiPF6、LiBF4、LiTFSI、LiAsF6、Li B(C2O4)2(Li BOB)、Li SO2CF3(Li
Tf) more than one.
2. the preparation method of the PEO base solid polymer electrolyte membranes described in a kind of claim 1, it is characterised in that specific
Preparation process is,
(1) preparation of blend solution
By PEO with 0.5~1.5:The solid-liquid ratio of 20~100g/ml is dissolved in dichloromethane, and is statically placed in iodine flask
12h, then by PMMA with 0.05~1：The solid-liquid ratio of 10~50g/ml is dissolved in dichloromethane, and dissolving is added to after stirring and dissolving is complete
In the dichloromethane solution of PEO, dissolving is stirred well to completely, the mass ratio of PEO and PMMA is 0.5~1.5 in mixed liquor：0
~1, then again to lithium perchlorate is added in mixed liquor, it is stirred at room temperature to dissolving fully, PEO is with the mass ratio of lithium perchlorate
0.5~1.5：0.01~1, it is put into rotor in iodine flask, sealing, at 25 DEG C, with 700rmp rotating speed magnetic agitations 90min；
(2) preparation of blend film
Weigh LCI/MMT hybrid material 1-METHYLPYRROLIDONEs and dissolving shaken in test tube, the solid-liquid ratio of the two be 0.001~
0.5:1~20g/ml, stirs to PEO/PMMA solution blendings obtained in addition step 1 in the solution of LCI/MMT, solid-liquid ratio
1~20:30~150g/ml, using automatic knifing machine knifing on a glass, blade thickness is 0.5mm, by obtained film drum
2h is dried at 50 DEG C of wind drying box, matrix, sealing preserve are peeled off with blade；
(3) cell package
Blend film obtained in step 2 is encapsulated into stainless steel battery, the composition material material of battery is stainless steel, before encapsulation
Ultrasonic oil removal is carried out using ultrasonic cleaner, encapsulation order is：Negative pole+shell fragment+pad+dielectric film+pad+pad+
Positive pole → small-sized hydraulic button cell packaging machine hydraulic pressure encapsulation.
3. the preparation method of PEO bases solid polymer electrolyte membrane according to claim 2, it is characterised in that in step 2
The structure of LCI is in LCI/MMT hybrid materials,
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108346822A (en) * | 2018-02-08 | 2018-07-31 | 广东猛狮新能源科技股份有限公司 | A kind of preparation method of 3D networks hybrid inorganic-organic all solid state electrolyte |
| CN109148818A (en) * | 2018-08-28 | 2019-01-04 | 江苏双登富朗特新能源有限公司 | Polyethylene oxide solutions filling technique for solid lithium battery |
| CN109449491A (en) * | 2018-10-18 | 2019-03-08 | 浙江众泰汽车制造有限公司 | A kind of preparation method and application of gel polymer electrolyte material |
| WO2019178972A1 (en) * | 2018-03-19 | 2019-09-26 | 深圳新宙邦科技股份有限公司 | Polymer electrolyte for lithium ion battery and polymer battery |
| CN110828906A (en) * | 2019-11-22 | 2020-02-21 | 四川贝克特瑞科技有限公司 | Preparation method and application of polymer-based solid electrolyte |
| CN111477951A (en) * | 2020-04-14 | 2020-07-31 | 宁德新能源科技有限公司 | Composite electrolyte and electrochemical and electronic device using the same |
| CN111525188A (en) * | 2020-05-14 | 2020-08-11 | 湘潭大学 | PEO-PMMA solid electrolyte membrane |
| CN113451645A (en) * | 2021-07-20 | 2021-09-28 | 武汉海翎化学工业有限公司 | High-conductivity polyethylene oxide electrolyte material and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108346822A (en) * | 2018-02-08 | 2018-07-31 | 广东猛狮新能源科技股份有限公司 | A kind of preparation method of 3D networks hybrid inorganic-organic all solid state electrolyte |
| WO2019178972A1 (en) * | 2018-03-19 | 2019-09-26 | 深圳新宙邦科技股份有限公司 | Polymer electrolyte for lithium ion battery and polymer battery |
| CN110289446A (en) * | 2018-03-19 | 2019-09-27 | 深圳新宙邦科技股份有限公司 | A kind of polymer dielectric and polymer battery for lithium ion battery |
| CN109148818A (en) * | 2018-08-28 | 2019-01-04 | 江苏双登富朗特新能源有限公司 | Polyethylene oxide solutions filling technique for solid lithium battery |
| CN109148818B (en) * | 2018-08-28 | 2021-04-13 | 江苏双登富朗特新能源有限公司 | Polyethylene oxide solution injection process for all-solid-state lithium battery |
| CN109449491A (en) * | 2018-10-18 | 2019-03-08 | 浙江众泰汽车制造有限公司 | A kind of preparation method and application of gel polymer electrolyte material |
| CN110828906A (en) * | 2019-11-22 | 2020-02-21 | 四川贝克特瑞科技有限公司 | Preparation method and application of polymer-based solid electrolyte |
| CN111477951A (en) * | 2020-04-14 | 2020-07-31 | 宁德新能源科技有限公司 | Composite electrolyte and electrochemical and electronic device using the same |
| CN111525188A (en) * | 2020-05-14 | 2020-08-11 | 湘潭大学 | PEO-PMMA solid electrolyte membrane |
| CN111525188B (en) * | 2020-05-14 | 2021-08-20 | 湘潭大学 | PEO-PMMA solid electrolyte membrane |
| CN113451645A (en) * | 2021-07-20 | 2021-09-28 | 武汉海翎化学工业有限公司 | High-conductivity polyethylene oxide electrolyte material and preparation method thereof |
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