CN115224359A - Polymer electrolyte, preparation method thereof and lithium ion all-solid-state battery - Google Patents
Polymer electrolyte, preparation method thereof and lithium ion all-solid-state battery Download PDFInfo
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- CN115224359A CN115224359A CN202210885723.9A CN202210885723A CN115224359A CN 115224359 A CN115224359 A CN 115224359A CN 202210885723 A CN202210885723 A CN 202210885723A CN 115224359 A CN115224359 A CN 115224359A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
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- 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
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Abstract
The invention provides a polymer electrolyte, a preparation method thereof and a lithium ion all-solid-state battery, wherein the polymer electrolyte comprises a continuous phase and a disperse phase, the preparation raw materials of the continuous phase comprise polyvinylpyrrolidone, polyethylene oxide and lithium bis (trifluoromethylsulfonyl) imide, and the preparation raw materials of the disperse phase comprise vinylene carbonate, lithium bis (trifluoromethylsulfonyl) imide and an initiator. The invention improves the ionic conductivity of the polymer electrolyte, simultaneously realizes the full contact of the polymer electrolyte and the electrode active material, effectively solves the problem of the interface between the polymer electrolyte membrane and the positive and negative pole pieces, and effectively improves the cycle performance of the all-solid-state battery.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a polymer electrolyte, a preparation method of the polymer electrolyte and a lithium ion all-solid-state battery.
Background
Compared with a liquid electrolyte system, the polymer electrolyte has many advantages, such as no leakage, easy miniaturization of devices, higher safety and the like. Earlier in the 20 th century, scholars discovered that inorganic solid-state electrolytes, such as AgI crystals, had super ionic conductivity at temperatures above the phase transition temperature (149 ℃) of the β -phase and a-phase, making the concept of "polymer electrolytes" practical in 1920 first; thereafter having a similarityThe crystalline super ionic conductor is continuously developed, and the room-temperature ionic conductivity reaches 10 -3 ～10 -4 Level of S/cm. However, the preparation of the inorganic solid electrolyte and the contact difference of the interface thereof are a large short plate; compared with the prior art, the polymer material has many excellent properties, such as good ductility, light weight, easy machining and the like, and the polymer electrolyte is rapidly developed in the field of lithium batteries due to the excellent properties of the polymer material.
The polymer electrolyte generally has excellent mechanical properties, can well inhibit the growth of lithium dendrites of a lithium metal negative electrode in the charging and discharging processes, and improves the safety performance of a lithium battery. Currently, polyethylene oxide (PEO) systems are widely studied in polymer electrolytes, but the high crystallinity thereof makes lithium ion migration difficult at room temperature, resulting in a problem of low ionic conductivity.
Moreover, after the all-solid-state battery is assembled, the interface resistance between the anode and the cathode and the electrolyte membrane is large, so that the capacity exertion of the all-solid-state battery is poor, and the cycle performance is poor.
Disclosure of Invention
The invention aims to develop a polymer electrolyte, a preparation method thereof and a lithium ion all-solid-state battery, so that the ionic conductivity of the polymer electrolyte is improved, the full contact between the polymer electrolyte and an electrode active material is realized, the problem of the interface between a polymer electrolyte membrane and positive and negative plates is effectively solved, and the cycle performance of the all-solid-state battery is effectively improved.
The invention is realized by the following technical scheme:
the invention relates to a preparation method of a polymer electrolyte, which comprises the following preparation steps:
s1, preparing a polymer electrolyte membrane: respectively weighing a certain amount of polyvinylpyrrolidone (PVP), polyethylene oxide (PEO) and lithium bis (trifluoromethylsulfonyl) imide (LiTFSI) to be dissolved in a good solvent to prepare a uniform solution, thereby obtaining the slurry of the polymer electrolyte. The electrolyte slurry is poured on a PTFE plate to form a film, and then the film is soaked in an ethanol solution for defoaming, so that the polymer electrolyte membrane with a porous structure is finally obtained.
S2, preparing a precursor solution: uniformly mixing vinylene carbonate and lithium bis (trifluoromethylsulfonyl) imide according to a certain proportion to form a uniform solution, adding an initiator, and slowly and uniformly stirring to prepare a precursor solution.
S3, preparing an in-situ polymer electrolyte: a certain amount (selected according to the size and pore diameter of the membrane) of the S2 precursor solution was dropped to the polymer electrolyte membrane prepared in S1 with a rubber-tipped dropper so as to fill the entire porous structure. Then placing the mixture in a vacuum oven for in-situ polymerization and peeling to obtain the polymer electrolyte.
Preferably, in S1, the mass ratio of the polyvinylpyrrolidone, the polyethylene oxide and the lithium bis (trifluoromethylsulfonyl) imide is (0.2-0.6) to (2-3.2) to (0.6-0.8).
Preferably, in S1, the good solvent is one of acetone, N-dimethylformamide and acetonitrile. Preferably, the good solvent is acetonitrile.
Preferably, the soaking time in ethanol in S1 is 1 min-20 min, and preferably, the soaking time in S1 is 5min.
Preferably, the molar ratio of vinylene carbonate to lithium bis (trifluoromethylsulfonyl) imide in S2 is (2-4): 1, and preferably, the molar ratio of vinylene carbonate to lithium bis (trifluoromethylsulfonyl) imide in S2 is 3.
Preferably, in S2, the initiator is one of azobisisobutyronitrile, azobisisoheptonitrile and dimethyl azobisisobutyrate. Preferably, the initiator in S2 is azobisisobutyronitrile.
Preferably, in S3, the in-situ polymerization temperature is 45-90 ℃, and the polymerization time is 1-3 h. Preferably, the polymerization temperature in S3 is 60 ℃ and the polymerization time is 2h.
The present invention also provides a polymer electrolyte comprising a polymer electrolyte membrane having a porous network structure and a dispersed phase filled in the porous network structure of the polymer electrolyte membrane; the polymer electrolyte membrane comprises a polyethylene oxide matrix, wherein polyvinylpyrrolidone and lithium bis (trifluoromethylsulfonyl) imide are crosslinked in the polyethylene oxide matrix; the dispersed phase is a polymer of vinylene carbonate and lithium bis (trifluoromethylsulfonyl) imide.
Preferably, in the polymer electrolyte membrane, the mass ratio of the polyvinylpyrrolidone, the polyethylene oxide and the lithium bis (trifluoromethylsulfonyl) imide is (0.2-0.6) to (2-3.2) to (0.6-0.8).
Preferably, the molar ratio of the vinylene carbonate to the lithium bis (trifluoromethylsulfonyl) imide in the dispersed phase is (2-4): 1.
The invention also provides a lithium ion all-solid-state battery which comprises a positive electrode, a negative electrode and the polymer electrolyte positioned between the positive electrode and the negative electrode.
Preferably, the positive electrode is obtained by coating positive electrode slurry on a current collector, and the preparation raw materials of the positive electrode slurry include: vinylene carbonate, lithium bis (trifluoromethylsulfonyl) imide, an initiator and a positive active material; the negative electrode is obtained by coating negative electrode slurry on a current collector, and the preparation raw materials of the negative electrode slurry comprise: vinylene carbonate, lithium bis (trifluoromethylsulfonyl) imide, an initiator and a negative active material.
The invention also provides a preparation method of the lithium ion all-solid-state battery, which comprises the following steps: adding a positive active substance into the precursor solution in the S2 as a solvent to prepare positive slurry, and then coating the positive slurry on a current collector to form a positive electrode; and (3) adding a negative active material into the precursor solution in the step (S2) as a solvent to prepare negative slurry, coating the negative slurry on a current collector to form a negative electrode, assembling the positive electrode and the negative electrode with the in-situ polymer electrolyte in the step (S3) to form a lithium battery, packaging, and then curing in situ to obtain the all-solid-state battery.
Preferably, the curing condition is that the curing temperature is 45-90 ℃ and the curing time is 1-3 h. Preferably, the curing temperature is 60 ℃ and the curing time is 2h.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the polymer electrolyte, the polyvinylpyrrolidone is crosslinked with the polyethylene oxide, so that the problem of high crystallinity of the polyethylene oxide polymer electrolyte is effectively solved, the ionic conductivity of the polymer electrolyte is improved, and the short plate of a PEO system is overcome. Meanwhile, the precursor solution of the electrolyte is filled in the polymer electrolyte membrane with the porous network structure, and the electrolyte remained in the porous network structure permeates into the interfaces and surfaces of the anode and the cathode in the manufacturing process of the battery, so that the electrolyte is distributed in the whole battery in a gradient manner, the interface impedance is effectively reduced, and the ion mobility is improved.
Furthermore, the invention prefers solvents, other polar solvents, which cannot prepare the desired electrolyte with porous structure.
The polymer electrolyte can reduce the crystallinity of the polyethylene oxide polymer electrolyte by using the polyvinylpyrrolidone to be crosslinked with the polyethylene oxide, thereby improving the ionic conductivity of the polymer electrolyte, and the maximum room-temperature ionic conductivity is more than 10 -4 S/cm, has higher ionic conductivity, and overcomes the defect of short plates of a PEO system. Meanwhile, the (trifluoromethyl sulfonyl) imide lithium is filled in the polymer electrolyte membrane and permeates into the interfaces and surfaces of the positive and negative electrodes in the manufacturing process of the battery, so that the electrolyte is distributed in the whole battery in a gradient manner, the interface impedance is effectively reduced, and the ion mobility is improved. Meanwhile, the polymer electrolyte improves the mechanical strength, widens the electrochemical window, has better corrosion resistance, is not easy to dissolve in an organic solvent, and can also be applied to a lithium battery with solid-liquid mixed electrolyte.
The lithium ion all-solid-state battery adopts the polymer electrolyte, the electrolyte filled in the polymer electrolyte permeates into the positive electrode and the negative electrode, so that slurry with the capability of conducting lithium ions is distributed in the whole solid-state battery in a gradient manner to construct an integrated structure, the problem of the interface between the polymer electrolyte membrane and the positive electrode and the negative electrode is effectively solved, and the cycle performance and the capacity performance of the all-solid-state battery are effectively improved.
Drawings
FIG. 1 is a macroscopic picture of a polymer electrolyte membrane with a porous network structure;
FIG. 2 is a picture of the corrosion resistance of a polymer electrolyte membrane;
fig. 3 is a discharge graph of an all-solid battery;
fig. 4 is a graph of a cycle curve for an all-solid-state battery.
Detailed Description
For a further understanding of the invention, reference will now be made to the following examples, which are provided to illustrate further features and advantages of the invention, and are not intended to limit the scope of the invention as set forth in the following claims.
Example 1, a preparation method and application of a polymer electrolyte:
step 1, preparation of a porous electrolyte membrane: 0.45g of PVP, 2.26g of PEO and 0.74g of LiTFSI0 are respectively weighed and dissolved in an acetonitrile solvent, the amount of acetonitrile is 13.8g, and the mixture is stirred for 4 hours at the rotating speed of 500rpm/min to form a uniform solution, so that slurry of the polymer electrolyte is obtained. The electrolyte slurry is poured on a PTFE plate to form a film, and then the film is soaked in ethanol for 5min for defoaming, so that a polymer electrolyte membrane with a porous structure is finally obtained, as shown in figure 1.
Step 2, preparation of precursor solution: weighing 22.63g of vinylene carbonate, putting the vinylene carbonate into a reactor, weighing 7.37g of lithium salt LiTFSI, adding the lithium salt LiTFSI into the reactor, weighing 0.02g of azobisisobutyronitrile into the reactor after the LiTFSI is completely dissolved in the vinylene carbonate, and slowly stirring until the LiTFSI is completely dissolved to form a uniform solution, thereby obtaining a precursor solution.
Step 3, preparing the in-situ polymer electrolyte: 10mL of the precursor solution was dropped to the polymer electrolyte membrane with a rubber-tipped dropper so as to fill the entire porous electrolyte membrane. And then placing the electrolyte in a vacuum oven for polymerization for 2 hours at 60 ℃ to obtain the in-situ polymer electrolyte.
And 4, taking the precursor solution prepared in the step 2 as a solvent to prepare slurry of a lithium iron phosphate anode and a graphite cathode, then coating the slurry on a current collector, assembling the lithium battery with the in-situ polymer electrolyte prepared in the step 3 filled with the precursor solution, packaging, curing in situ for 2 hours at 60 ℃ to obtain an all-solid-state battery 1, and then keeping the temperature constant for 22 hours and starting testing.
Example 2
Step 1, preparation of a porous electrolyte membrane: 0.6g of PVP, 3.2g of PEO and 0.8g of LiTFSI are respectively weighed and dissolved in an acetonitrile solvent, the amount of acetonitrile is 13.8g, and the mixture is stirred for 4 hours at the rotating speed of 500rpm/min to form a uniform solution, so that slurry of the polymer electrolyte is obtained. The electrolyte slurry is poured on a PTFE plate to form a film, and then the film is soaked in ethanol for 5min for defoaming, so that a polymer electrolyte membrane with a porous structure is finally obtained, as shown in figure 1.
Step 2, preparation of precursor solution: weighing 22.63g of vinylene carbonate into a reactor, weighing 7.37g of lithium salt LiTFSI into the reactor, weighing 0.02g of azobisisobutyronitrile into the reactor after the LiTFSI is completely dissolved in the vinylene carbonate, and slowly stirring until the LiTFSI is completely dissolved to form a uniform solution, thereby obtaining a precursor solution.
Step 3, preparing the in-situ polymer electrolyte: 10mL of the precursor solution was dropped to the polymer electrolyte membrane with a rubber-tipped dropper so as to fill the entire porous electrolyte membrane. Then placing the mixture in a vacuum oven for polymerization for 3 hours at the temperature of 45 ℃ to obtain the in-situ polymer electrolyte.
And 4, taking the precursor solution prepared in the step 2 as a solvent to prepare slurry of the lithium iron phosphate anode and the graphite cathode, then coating the slurry on a current collector, assembling the lithium battery with the in-situ polymer electrolyte prepared in the step 3 filled with the precursor solution, packaging, curing in situ for 3 hours at 45 ℃ to obtain an all-solid-state battery 2, and keeping the temperature constant for 22 hours and then starting testing.
Example 3
Step 1, preparation of a porous electrolyte membrane: PVP 0.2g, PEO 2.0g and LiTFSI 0.6g are respectively weighed and dissolved in an acetonitrile solvent, the amount of acetonitrile is 13.8g, and the mixture is stirred for 4 hours at the rotating speed of 500rpm/min to form a uniform solution, so that slurry of the polymer electrolyte is obtained. The electrolyte slurry is poured on a PTFE plate to form a film, and then the film is soaked in ethanol for 5min for defoaming, so that a polymer electrolyte membrane with a porous structure is finally obtained, as shown in figure 1.
Step 2, preparation of precursor solution: weighing 22.63g of vinylene carbonate, putting the vinylene carbonate into a reactor, weighing 7.37g of lithium salt LiTFSI, adding the lithium salt LiTFSI into the reactor, weighing 0.02g of azobisisobutyronitrile into the reactor after the LiTFSI is completely dissolved in the vinylene carbonate, and slowly stirring until the LiTFSI is completely dissolved to form a uniform solution, thereby obtaining a precursor solution.
Step 3, preparing the in-situ polymer electrolyte: 10mL of the precursor solution was dropped to the polymer electrolyte membrane with a rubber-tipped dropper so as to fill the entire porous electrolyte membrane. Then placing the mixture in a vacuum oven to polymerize for 1h at 90 ℃ to obtain the in-situ polymer electrolyte.
And 4, taking the precursor solution prepared in the step 2 as a solvent to prepare slurry of a lithium iron phosphate anode and a graphite cathode, then coating the slurry on a current collector, assembling the lithium battery with the in-situ polymer electrolyte prepared in the step 3 filled with the precursor solution, packaging, curing in situ for 1h at 90 ℃ to obtain an all-solid-state battery 3, and then keeping the temperature constant for 22h and starting testing.
Comparative example 1
Step 1, weighing 2.3g of polymer PEO and 0.7g of lithium salt LiTFSI, slowly adding the polymer PEO and the lithium salt LiTFSI into acetonitrile serving as a solvent, wherein the using amount of the acetonitrile is 13.8g, and magnetically stirring the mixture for 5 hours at the rotating speed of 500rpm/min to obtain polymer electrolyte slurry. And pouring the prepared slurry on a PTFE (polytetrafluoroethylene) mold, placing the PTFE mold in a drying room, and airing to prepare the nonporous polymer electrolyte. And assembling the negative electrode shell, the gasket, the polymer electrolyte, the gasket, the elastic sheet and the positive electrode shell into a button cell in sequence, and testing the ionic conductivity of the button cell at the conditions of 25 ℃, 45 ℃, 65 ℃ and 85 ℃.
Step 2, mixing the prepared polymer electrolyte and LFP (LiFePO) 4 ) And a metallic lithium negative electrode were assembled into an all-solid battery 2, and subjected to an electrochemical performance test. At 60 ℃, 3.65V-2.5V and 0.2C, the all-solid battery 2 can not be charged and discharged normally, which is probably caused by poor physical contact between the anode and the cathode and the polymer electrolyte membrane and larger internal resistance.
The polymer electrolyte membrane of example 1 was subjected to a corrosion test, and the corrosion solution was an electrolyte solution prepared from 1M lithium hexafluorophosphate and dimethyl carbonate/ethylene carbonate/ethyl methyl carbonate (mass ratio 1.
The ionic conductivities of the polymer electrolytes obtained in examples 1 to 3 and comparative example 1 were measured, and as a result, as shown in table 1, it can be seen that the ionic conductivities of the polymer electrolytes of examples 1 to 3 were significantly higher than that of the polymer electrolyte of comparative example 1, indicating that the addition of PVP can improve the ionic conductivity of the polymer electrolyte.
TABLE 1 Absolute value of ion conductivity of Polymer electrolyte Membrane
| Comparative example 1 | Example 1 | Example 2 | Example 3 | |
| 25℃ | 4.16E-06 | 1.05E-04 | 8.16E-06 | 5.23E-06 |
| 45℃ | 4.53E-05 | 6.15E-04 | 6.3E-05 | 4.83E-05 |
| 65℃ | 3.58E-04 | 2.66E-03 | 5.85E-04 | 3.94E-04 |
| 85℃ | 8.05E-04 | 6.37E-03 | 9.1E-04 | 9.17E-04 |
The all-solid-state batteries 1 and 2 prepared in example 1 and comparative example 1 were subjected to an electrical property test, and their cycle properties and charge and discharge properties were measured. Fig. 3 is a discharge curve diagram of the solid-state batteries of comparative example 1 and example 1, and it can be seen from fig. 3 that the discharge energy of the all-solid-state battery prepared in example 1 reaches 152mAh/g at 0.2C discharge current, and the all-solid-state battery has a discharge plateau of 3.4V and a charge-discharge curve of a standard lithium iron phosphate material, and compared with the solid-state battery of comparative example 1, the all-solid-state battery of example 1 has a discharge capacity of 30mAh/g, has good discharge capacity, and is close to the theoretical discharge energy of the lithium iron material. Fig. 4 is a graph showing the cycle performance of the solid-state batteries of comparative example 1 and example 1, and it can be seen from fig. 4 that the 0.2C cycle 30cycle capacity retention rate of the solid-state battery of example 1 reaches 99.8%, and the 0.2C cycle 30cycle capacity retention rate of the solid-state battery of comparative example 1 is less than 40%, which fully illustrates that the solid-state battery prepared in example 1 has reversible lithium intercalation capacity and excellent cycle performance.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (10)
1. A method for producing a polymer electrolyte, comprising:
s1, dissolving polyvinylpyrrolidone, polyethylene oxide and lithium bis (trifluoromethylsulfonyl) imide in a good solvent to obtain electrolyte slurry, and pouring the electrolyte slurry on a substrate to form a film to obtain a polymer electrolyte film with a porous structure;
s2, uniformly mixing vinylene carbonate, lithium bis (trifluoromethylsulfonyl) imide and an initiator to obtain a precursor solution;
and S3, dropwise adding the precursor solution onto the polymer electrolyte membrane to enable the precursor solution to fill the pores in the polymer electrolyte membrane and carry out in-situ polymerization, and then stripping the polymer electrolyte membrane from the substrate to obtain the polymer electrolyte.
2. The method for producing a polymer electrolyte according to claim 1, wherein the good solvent in S1 is one of acetone, N-dimethylformamide, and acetonitrile.
3. The method of claim 1, wherein in S2, the initiator is one of azobisisobutyronitrile, azobisisoheptonitrile, and dimethyl azobisisobutyrate.
4. The method for preparing a polymer electrolyte according to claim 1, wherein the mass ratio of polyvinylpyrrolidone, polyethylene oxide and lithium bis (trifluoromethylsulfonyl) imide in S1 is (0.2-0.6) to (2-3.2) to (0.6-0.8); in S2, the molar ratio of vinylene carbonate to lithium bis (trifluoromethylsulfonyl) imide is (2-4): 1.
5. The method for preparing a polymer electrolyte according to claim 1, wherein the in-situ polymerization in S3 is performed at a temperature of 45 ℃ to 90 ℃ for 1 hour to 3 hours.
6. A polymer electrolyte characterized by comprising a polymer electrolyte membrane having a porous network structure and a dispersed phase filled in the porous network structure of the polymer electrolyte membrane; the polymer electrolyte membrane comprises a polyethylene oxide matrix, wherein polyvinylpyrrolidone and lithium bis (trifluoromethylsulfonyl) imide are crosslinked in the polyethylene oxide matrix; the dispersed phase is a polymer of vinylene carbonate and lithium bis (trifluoromethylsulfonyl) imide.
7. The method for producing a polymer electrolyte according to claim 6, wherein the mass ratio of polyvinylpyrrolidone, polyethylene oxide and lithium bis (trifluoromethanesulfonyl) imide in the polymer electrolyte membrane is (0.2-0.6): (2-3.2): (0.6-0.8).
8. The method for producing a polymer electrolyte according to claim 6, wherein the molar ratio of vinylene carbonate to lithium bis (trifluoromethylsulfonyl) imide in the dispersed phase is (2 to 4): 1.
9. A lithium ion all-solid-state battery comprising a positive electrode, a negative electrode, and the polymer electrolyte according to any one of claims 6 to 8 or the polymer electrolyte obtained by the production method according to any one of claims 1 to 5, which is interposed between the positive electrode and the negative electrode.
10. The lithium ion all-solid battery according to claim 8, wherein the positive electrode is obtained by coating a positive electrode slurry on a current collector and curing, and the positive electrode slurry comprises: vinylene carbonate, lithium bis (trifluoromethylsulfonyl) imide, an initiator and a positive active material; the negative electrode is obtained by coating negative electrode slurry on a current collector and solidifying, and the negative electrode slurry comprises: vinylene carbonate, lithium bis (trifluoromethylsulfonyl) imide, an initiator and a negative active material.
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| CN116130755A (en) * | 2022-11-14 | 2023-05-16 | 吉林省东驰新能源科技有限公司 | Self-supporting polyethylene carbonate electrolyte, preparation method and application thereof, and room-temperature all-solid-state lithium ion battery |
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| CN116130755A (en) * | 2022-11-14 | 2023-05-16 | 吉林省东驰新能源科技有限公司 | Self-supporting polyethylene carbonate electrolyte, preparation method and application thereof, and room-temperature all-solid-state lithium ion battery |
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