CN114094176A - Gel electrolyte diaphragm treatment method - Google Patents

Gel electrolyte diaphragm treatment method Download PDF

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Publication number
CN114094176A
CN114094176A CN202111339444.4A CN202111339444A CN114094176A CN 114094176 A CN114094176 A CN 114094176A CN 202111339444 A CN202111339444 A CN 202111339444A CN 114094176 A CN114094176 A CN 114094176A
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solvent
gel electrolyte
diaphragm
glycol dimethyl
battery
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刘喜正
耿慧
丁轶
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Tianjin University of Technology
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Tianjin University of Technology
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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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403—Manufacturing processes of separators, membranes or diaphragms
    • 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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  • Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Dispersion Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Secondary Cells (AREA)
  • Cell Separators (AREA)

Abstract

The invention relates to a processing method of a gel electrolyte diaphragm. The method comprises the following steps: adding an initiator into an organic solvent, and mixing to obtain a prefabricated solution; coating the prefabricated solution obtained in the previous step on the surface of a diaphragm, and standing for 0.1-10 days to obtain the diaphragm with the initiator; and (3) dropwise adding electrolyte on the surface of the diaphragm with the initiator obtained in the previous step, standing for 0.1-10 days to form a polymer gel electrolyte in situ, and thus obtaining the battery diaphragm. The initiator is Lewis acid. The method is simple, low in cost, practical and effective.

Description

Gel electrolyte diaphragm treatment method
Technical Field
The invention relates to a processing method of a gel electrolyte and application thereof, in particular to a preparation method of an in-situ gel electrolyte in a battery and application thereof in the battery, belonging to the related field of secondary batteries.
Background
In recent years, new secondary batteries such as lithium ion batteries and sodium ion batteries are increasingly used in production and life of people, and batteries of gel polymer electrolyte systems meet the requirements of people on high energy density, safety and flexible devices. However, most of the current preparation methods of gel electrolytes are relatively complex, and the formation of a plurality of gel materials requires specific conditions. CN 102670567A discloses a preparation method of a flame-retardant gel electrolyte, the prepared non-hydrogel electrolyte needs to initiate polymerization reaction under high temperature condition to prepare the gel electrolyte, the preparation process is complex, and the time consumption is long; CN 113258131 a discloses a preparation method of a gel polymer electrolyte, which needs to be left standing at 60 ℃ for 24 hours to form the gel electrolyte; CN 113270641A prepares gel electrolyte under the condition of ultraviolet irradiation, and the method is complex and the gelling condition is harsh. (DOI:10.1126/sciadv. aat5383) states that the preparation of gel electrolytes by ring-opening polymerization of 1, 3-dioxane using lithium salts at a concentration of 2 moles per liter is expensive, and the cost is multiplied by the high concentration of lithium salts, so that the selection of non-lithium salts, low concentration, and inexpensive initiators is a necessary condition for commercial application.
Disclosure of Invention
The invention aims to solve the problems and provide a method for treating a separator with surface initiated Lewis acid. According to the method, a Lewis acid initiator is coated on the surface of a diaphragm through a prefabricated solution, then an electrolyte is dripped to assemble the battery, and ring-opening polymerization of cycloalkane is induced, so that the electrolyte realizes in-situ gelation under the induction of the initiator on the diaphragm, an in-situ gel electrolyte is obtained in the battery, and the phenomenon of polymer plasticization is improved. The method is simple, low in cost, practical and effective.
The technical scheme of the invention is as follows:
a gel electrolyte membrane treatment method comprising the steps of:
(1) adding an initiator into an organic solvent, and mixing to obtain a prefabricated solution;
wherein the volume of the initiator is 0.1-30% of that of the organic solvent;
the initiator is Lewis acid;
the Lewis acid aluminum trichloride, boron trifluoride diethyl etherate, sulfur trioxide, ferric bromide, stannic chloride, titanium tetrachloride, ferric trichloride, scandium trifluoromethanesulfonate, tert-butyl hydroperoxide, p-chlorobenzene sulfonic acid or boron phosphoric acid;
the organic solvent is an ether solvent, an ester solvent, a hydrocarbon solvent, a sulfone solvent or other solvents;
the ester solvent is dimethyl carbonate, diethyl carbonate, ethylene carbonate or propylene carbonate;
the ether solvent is ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, dioxolane or tetrahydrofuran;
the hydrocarbon solvent is n-butane, toluene, xylene, dichloromethane or dichloroethane;
the sulfone solvent is dimethyl sulfoxide, ethyl dimethyl sulfone or tetramethyl sulfone;
the other solvent is acetonitrile, pyridine or various ionic liquids.
(2) Coating the prefabricated solution obtained in the previous step on the surface of a diaphragm, and standing for 0.1-10 days to obtain the diaphragm with the initiator; coating 0.01-10 ml of prefabricated solution on the surface of the diaphragm per square centimeter;
the surface of the membrane may be single-sided or double-sided.
(3) Dropwise adding electrolyte on the surface of the diaphragm with the initiator obtained in the previous step, standing for 0.1-10 days to form polymer gel electrolyte in situ, and obtaining a battery diaphragm;
the volume of the electrolyte dripped on the surface of the diaphragm per square centimeter is 1-10 times of the volume of the prefabricated solution.
The electrolyte is a metal salt solution, and the concentration of the electrolyte is 0.1-3.0M; the solvent is one or more of an ether solvent and cyclane; when the two mixed solutions are adopted, the volume ratio of the two mixed solutions is 1: 100-100: 1,
the metal salt is one or more of lithium salt, sodium salt and potassium salt;
the ether solvent is one or more of ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether and tetraethylene glycol dimethyl ether.
The cycloalkane is 1, 3-dioxane, tetrahydrofuran, 1,3, 5-trioxane, 1, 3-dioxolane cyclopropane, cyclobutane, cyclopentane, cyclohexane and other monocyclic, bicyclic, tricyclic or polycyclic alkyl substituted derivatives;
the metal salt solutionThe medium lithium salt is LiPF6、LiBF4、LiCl、LiAlCl、LiSbF6、LiSCN、LiClO4、LiCF3SO3、LiCF3CO2、LiN(CF3SO2)2、LiAsF6、LiBC4O8、LiN(FSO2)2LiTFSI or LiOTf; the sodium salt is NaPF6、NaBF6、NaCl、NaAlCl、NaSbF6、NaSCN、NaClO4、NaCF3SO3、NaCF3CO2、NaN(CF3SO2)2、NaAsF6、NaBC4O8、NaN(FSO2)2NaTFSI or NaOTf; the sylvite is KPF6、KBF6、KCl、KAlCl、KSbF6、KSCN、KClO4、KCF3SO3、KCF3CO2、KN(CF3SO2)2、KAsF6、KBC4O8、KN(FSO2)2KTFSI or KOTf.
The membrane is made of Polyolefin (polyofefin) membranes or Glass fiber (Glass fiber) membranes;
the polyolefin is Polyethylene (PE) or polypropylene (PP).
The separator with the surface provided with the initiating Lewis acid is applied to be used as a separator in a battery.
The battery is preferably a button cell battery and a soft package battery.
The invention has the beneficial effects that:
the invention adopts a simple method to prepare the diaphragm with low-concentration ring-opening initiator (Lewis acid), firstly prepares the diaphragm with initiating Lewis acid on the surface, and after the battery is assembled with an electrolyte, the electrolyte is gelated in situ in the standing process of the battery, thus obtaining the in-situ gel electrolyte. The capacity of the lithium-sulfur battery assembled by using the gel electrolyte is kept at 650 mAmp-1 after 100 cycles, and the attenuation of the capacity of the common electrolyte is serious, so that in a metal cation battery system, the shuttle effect of polysulfide in the lithium-sulfur battery system is effectively solved, the electrochemical window of the electrolyte is improved, and the cycle stability of the battery is improved.
The diaphragm obtained by the invention has excellent electrochemical performance, and the preparation method is simple, and the raw materials are easy to obtain, prepare and store; particularly, the cost of the battery can be obviously reduced, and compared with the button battery with the same model, the consumption of the electrolyte can be saved by more than 50 percent.
Drawings
Fig. 1 is an optical photograph of a gel electrolyte formed by in-situ gelation of the separator having an initiating lewis acid on the surface obtained in example 1.
Fig. 2 is a cycle performance curve of a lithium-lithium symmetric battery having a separator with an initiating lewis acid on the surface thereof formed as a gel electrolyte separator by in-situ gelation, obtained in example 1.
Fig. 3 is a graph comparing the cycle performance curves of the lithium sulfur battery having the separator with an initiating lewis acid on the surface obtained in example 1 and the conventional electrolyte separator in comparative example 1.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
1) mixing ethylene glycol dimethyl ether and boron trifluoride diethyl etherate solvent according to the volume ratio of 10:1 to obtain a prefabricated solution with an initiator;
2) coating the single side of a common polypropylene diaphragm with the prefabricated solution, and assembling the battery after volatilizing DME; wherein 7.06 milliliters of the pre-prepared solution is coated on each square centimeter of the diaphragm;
3) preparing an electrolyte, wherein the solvent is 1, 3-dioxane and ethylene glycol dimethyl ether, and the volume ratio of the 1, 3-dioxane to the ethylene glycol dimethyl ether is as follows: ethylene glycol dimethyl ether is 7:3, and solutes are lithium salt LiTFSI and LiNO3LiTFSI at a concentration of 1M (mol/l) and LiNO at a concentration of 0.1M3；
4) And (3) dropwise adding electrolyte into the diaphragm obtained in the step (2), assembling the diaphragm with a positive electrode and a negative electrode to form a battery, wherein one side of the diaphragm with the surface having initiating Lewis acid faces the positive electrode, 3.09 microliters of electrolyte obtained in the step (3) is dropwise added onto the surface of each square centimeter of the two sides of the diaphragm, metal lithium is used as a negative electrode piece, and a carbon-sulfur electrode is used as a positive electrode piece. And assembling the lithium-sulfur battery, standing for about 6 hours to obtain the gel electrolyte diaphragm formed by in-situ gelation of the diaphragm with the surface having the initiating Lewis acid. In particular to a CR2032 button cell.
The preparation method of the positive pole piece in the step 4) comprises the following steps:
1. carbon nano tubes (the mass percentage of the sulfur-carbon composite material is 23 percent) and sublimed sulfur (the mass percentage of the sulfur-carbon composite material is 77 percent), and the sulfur is melted at high temperature (155 ℃ C.) to prepare the sulfur-carbon composite material.
2. Preparing a positive electrode material, wherein the sulfur-carbon composite material accounts for 80% of the total mass of the positive electrode material in the step 1, the conductive agent carbon black (KB) accounts for 10% of the total mass of the positive electrode material, and the binder polyvinylidene fluoride (PVDF) accounts for 10% of the total mass of the positive electrode material; then adding a dispersing agent N-methyl pyrrolidone (1.5 ml of dispersing agent is added to each g of the positive electrode material) into the mixed positive electrode material, uniformly mixing to obtain slurry, coating the slurry on a current collector, drying the electrode in a vacuum oven at 55 ℃ for 8 hours, taking out the electrode, and cutting the electrode into a wafer with the radius of 5 mm to be used as a battery positive electrode, wherein the thickness of attachments of the electrode is 30 microns, and the sulfur loading capacity is 1 mg/square centimeter.
FIG. 1 is an optical photograph of in situ gelation of a separator having an initiating Lewis acid on the surface. The low concentration initiating electrolyte in situ gel had a very significant effect, and it can be clearly seen that the boron trifluoride treated Celgard separator can gel significantly outside the cell, with the bright place being the stable gel electrolyte formed.
Fig. 2 is a graph of the long cycle performance of a lithium-lithium symmetric cell with gel electrolyte at a current of 0.5 milliamps per square centimeter, with the abscissa representing test time and the ordinate representing voltage in V (volts). The polarized voltage is about 0.1V, and the stable cycle can be more than 1400 hours, which shows the inhibition effect of the gel electrolyte diaphragm on the dendritic growth of the metal cathode and the improvement on the long cycle performance.
Comparative example 1:
the other steps are the same as step 4) in example 1, except that an untreated ordinary polypropylene diaphragm was used;
the electrolyte used was the same as that used in step 3) of example 1, and 6.18. mu.l of the electrolyte obtained in step 3) of example 1 was dropped on both sides of the diaphragm per square centimeter of the surface. And finally obtaining the CR2032 button cell.
The cycle performance curves of the lithium sulfur battery having the separator with an initiating lewis acid on the surface obtained in example 1 and the conventional electrolyte separator in comparative example 1 are shown in fig. 3, where the abscissa represents the number of cycles and the ordinate represents the specific capacity in milliamp-hours/gram. It can be seen that in example 1, a gel electrolyte cell formed by in-situ gelation of a separator having an initiating lewis acid on the surface thereof under a 0.5C (1C: 1675 milliampere-hour/gram) current condition, after stable circulation for 100 circles, the capacity is attenuated to about 600 mAmp hours/g from 1000 mAmp hours/g, in comparative example 1, the capacity of the conventional liquid electrolyte battery was decreased from 1000 mAmp-hr/g to about 450 mAmp-hr/g after stable cycling for 100 cycles, and after 100 cycles of long cycling, compared to the conventional liquid electrolyte battery in example 1, the gel electrolyte formed by the membrane in-situ gelation with the surface having the initiating Lewis acid has higher capacity retention rate, the electrolyte consumption is reduced by one time, the capacity is reduced by one fourth and is continuously attenuated, which shows that the gel electrolyte has a barrier effect on polysulfide shuttle effect and improves the long cycle performance.
Example 2
The other steps are the same as the example 1, except that the position of the boron trifluoride preformed solution processing diaphragm in the step 2) is changed into two-side processing diaphragms, the coating amount of each side diaphragm in unit area is the same and is consistent with the example 1, and the electrolyte is guided to be gelled in situ after the diaphragm is processed. Comparative example the other steps were the same as in comparative example 1.
When the electrolyte is applied to a lithium-sulfur battery system under the current of 0.5C (1C: 1675 mAmp hour/g), the capacity of a gel electrolyte battery formed by the in-situ gelation of a diaphragm with initiating Lewis acid on both sides is reduced to about 700 mAmp hour/g from 990 mAmp hour/g after 100 circles of stable circulation, 3.09 microliters of the electrolyte obtained in the step 3) of the embodiment 1 is dripped on each square centimeter of surface on both sides of the diaphragm, compared with the capacity of the common liquid electrolyte, the capacity is reduced to about 450 mAmp hour/g from 1000 mAmp hour/g,
the amount of electrolyte is one time of that of the gel electrolyte after the separator is treated by the Lewis acid, and the capacity attenuation is two times of that of the gel electrolyte.
Example 3
The other steps are the same as example 1 except that the step 5) is carried out so that the sulfur capacity of the positive electrode is 2.5 mg/cm, the amount of the gel electrolyte formed by the membrane in-situ gelation with the lewis acid on the surface is still 3.09 μ l/cm under the current of 0.5C (1C: 1675 ma hour/g), the conditions are the same as those of comparative example 1 except that the positive electrode material is the step 5) carried out in example 1, and in the lithium-sulfur battery system, the capacity of the battery system formed by the membrane in-situ gelation with the lewis acid as the electrolyte is reduced from 1300 ma hour/g to 600 ma hour/g after 100 cycles of stable cycle, compared with the common liquid electrolyte battery system, the capacity is kept at 400 ma hour/g all the time, and the practical application value is not possessed, so that the amount of the gel electrolyte formed by the membrane in-situ gelation with the lewis acid as the electrolyte is less than that of the common electrolyte The consumption is 33.3%, the cost is saved, and the cycle performance of the battery is improved.
The invention is not the best known technology.

Claims (9)

1. A gel electrolyte membrane treatment method, characterized in that the method comprises the steps of:
(1) adding an initiator into an organic solvent, and mixing to obtain a prefabricated solution;
wherein the volume of the initiator is 0.1-30% of that of the organic solvent;
the initiator is Lewis acid;
the organic solvent is an ether solvent, an ester solvent, a hydrocarbon solvent, a sulfone solvent or other solvents;
(2) coating the prefabricated solution obtained in the previous step on the surface of a diaphragm, and standing for 0.1-10 days to obtain the diaphragm with the initiator; coating 0.01-10 ml of prefabricated solution on the surface of the diaphragm per square centimeter;
(3) dropwise adding electrolyte on the surface of the diaphragm with the initiator obtained in the previous step, standing for 0.1-10 days to form polymer gel electrolyte in situ, and obtaining a battery diaphragm;
the volume of the electrolyte dripped on the surface of the diaphragm per square centimeter is 1-10 times of the volume of the prefabricated solution.
2. The gel electrolyte membrane treatment method as claimed in claim 1, wherein the lewis acid is aluminum trichloride, boron trifluoride diethyl ether, sulfur trioxide, iron bromide, tin tetrachloride, titanium tetrachloride, iron trichloride, scandium trifluoromethanesulfonate, t-butyl hydroperoxide, p-chlorobenzenesulfonic acid, or borophosphoric acid.
3. The gel electrolyte membrane treatment method as claimed in claim 1, wherein the ester-based solvent is dimethyl carbonate, diethyl carbonate, ethylene carbonate or propylene carbonate;
the ether solvent is ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, dioxolane or tetrahydrofuran;
the hydrocarbon solvent is n-butane, toluene, xylene, dichloromethane or dichloroethane;
the sulfone solvent is dimethyl sulfoxide, ethyl dimethyl sulfone or tetramethyl sulfone;
the other solvent is acetonitrile, pyridine or various ionic liquids.
4. The gel electrolyte membrane treatment method as claimed in claim 1, wherein the surface of the membrane may be single-sided or double-sided.
5. The method of treating a gel electrolyte separator according to claim 1, wherein the separator is made of a polyolefin-based separator or a glass fiber-based separator; the polyolefin is polyethylene or polypropylene.
6. The method for treating a gel electrolyte membrane as claimed in claim 1, wherein the electrolyte is a metal salt solution having a concentration of 0.1 to 3.0M; the solvent is one or more of an ether solvent and a cyclic alkyl solvent; when the two mixed solutions are adopted, the volume ratio of the two mixed solutions is 1: 100-100: 1,
the metal salt is one or more of lithium salt, sodium salt and potassium salt.
7. The method for treating a gel electrolyte membrane according to claim 6, wherein the ether solvent is one or more selected from the group consisting of ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether and tetraethylene glycol dimethyl ether.
The cycloalkane is one or more of 1, 3-dioxane, tetrahydrofuran, 1,3, 5-trioxane, 1, 3-dioxolane cyclopropane, cyclobutane, cyclopentane, cyclohexane and other monocyclic, bicyclic, tricyclic or polycyclic alkyl substituted derivatives.
8. The gel electrolyte membrane treatment method as claimed in claim 6, wherein the lithium salt in the metal salt solution is LiPF6、LiBF4、LiCl、LiAlCl、LiSbF6、LiSCN、LiClO4、LiCF3SO3、LiCF3CO2、LiN(CF3SO2)2、LiAsF6、LiBC4O8、LiN(FSO2)2LiTFSI or LiOTf; the sodium salt is NaPF6、NaBF6、NaCl、NaAlCl、NaSbF6、NaSCN、NaClO4、NaCF3SO3、NaCF3CO2、NaN(CF3SO2)2、NaAsF6、NaBC4O8、NaN(FSO2)2NaTFSI or NaOTf; the sylvite is KPF6、KBF6、KCl、KAlCl、KSbF6、KSCN、KClO4、KCF3SO3、KCF3CO2、KN(CF3SO2)2、KAsF6、KBC4O8、KN(FSO2)2KTFSI or KOTf.
9. Use of the gel electrolyte separator prepared by the method according to claim 1, characterized in that it is used as a separator in a battery; the battery is preferably a button cell battery and a soft package battery.
CN202111339444.4A 2021-11-12 2021-11-12 Gel electrolyte diaphragm treatment method Pending CN114094176A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN115954609A (en) * 2023-01-16 2023-04-11 江苏正力新能电池技术有限公司 Spinning diaphragm, manufacturing method thereof and lithium battery

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JP2001273925A (en) * 2000-03-28 2001-10-05 Nof Corp Electrolyte for secondary battery and secondary battery
CN101622750A (en) * 2007-05-15 2010-01-06 株式会社Lg化学 Secondary battery and manufacturing method of the same
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Publication number Priority date Publication date Assignee Title
CN115954609A (en) * 2023-01-16 2023-04-11 江苏正力新能电池技术有限公司 Spinning diaphragm, manufacturing method thereof and lithium battery

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