CN114430062B - Composite electrolyte based on lithiated carbon point modification and preparation method and application thereof - Google Patents
Composite electrolyte based on lithiated carbon point modification and preparation method and application thereof Download PDFInfo
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- CN114430062B CN114430062B CN202210078871.XA CN202210078871A CN114430062B CN 114430062 B CN114430062 B CN 114430062B CN 202210078871 A CN202210078871 A CN 202210078871A CN 114430062 B CN114430062 B CN 114430062B
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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
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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
- H01M10/052—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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- 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
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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
Abstract
The invention provides a composite electrolyte based on lithiated carbon point modification, a preparation method and application thereof, wherein the composite electrolyte comprises a polymer electrolyte and an interface layer on the surface of the polymer electrolyte, and the interface layer comprises LiF; the polymer electrolyte comprises a high molecular polymer, lithium salt and lithiated carbon points; the lithiated carbon point is obtained by reacting acetaldehyde with a lithium precursor under alkaline conditions, wherein the lithium precursor comprises lithium bis (trifluoromethanesulfonyl) imide and/or lithium trifluorosulfonyl imide. According to the invention, the specific lithiated carbon points are added into the conductive polymer, so that an interface layer is formed on the surface of the composite electrolyte in the use process, the migration number of lithium ions and the ionic conductivity are improved, meanwhile, the interface can be stabilized, the rapid transmission of ions is facilitated, and the problem of dendrite generation due to uneven deposition is effectively solved.
Description
Technical Field
The invention relates to the technical field of solid electrolyte preparation, in particular to a lithiated carbon point modified composite electrolyte, and a preparation method and application thereof.
Background
The arrival of the carbon neutralization age means the profound change of human society productivity, and brings profound influence to various industries. The use of clean energy can overcome the challenges presented by traditional fossil energy while achieving the dual carbon goal. Lithium ion secondary batteries in energy storage technology have been widely used in many aspects of human life due to their own advantages, for example: 3C electronic products, electric automobiles, large-scale energy storage and the like.
The energy revolution has further driven the explosive development of lithium ion batteries. However, the development of modern society places higher demands on lithium ion batteries: a higher energy density and higher safety are required. The traditional lithium ion battery based on liquid electrolyte has the defects of low specific capacity of a negative electrode, unsafe hidden danger of carbonate electrolyte and the like, and needs to develop a new battery system. All-solid-state battery systems have the advantages of matching lithium metal (high specific capacity, low potential), no organic electrolyte (safety), and the like, and are considered as one of the most potential next-generation battery systems. The solid electrolytes in the solid electrolytes are classified into two types: inorganic solid electrolytes and polymer solid electrolytes. The polymer solid electrolyte has high flexibility and low cost, is suitable for the traditional battery winding technology, and has good application prospect.
However, the low ionic conductivity of the polymer electrolyte has limited its development, while low lithium ion transfer number is a limiting factor for the high performance of the full cell. The construction of a composite electrolyte by adding inorganic electrolyte particles as a filler is one of the effective methods for improving ion transport, but the difference in dispersibility of inorganic electrolyte and high molecular polymer in a solvent is a problem to be solved for preparing a high quality composite electrolyte. In order to increase the ion transfer number and the ion conductivity of the solid electrolyte, there is a mention in the prior art of preparing a solid electrolyte by mixing carbon dots with a polymer to increase the ion transfer number and the ion conductivity. However, the current polymer electrolyte still has the condition that lithium dendrites are generated due to uneven deposition of a lithium metal interface of a negative electrode in the use process, so that the cycle performance and the service life of the battery are affected.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides the composite electrolyte based on the modification of the lithiated carbon points, and the specific lithiated carbon points are added into the conductive polymer, so that an interface layer is formed on the surface of the composite electrolyte in the use process, the migration number of lithium ions and the ion conductivity are improved, the interface can be stabilized, the rapid ion transmission is assisted, and the problem of dendrite generation due to uneven deposition is effectively solved.
In order to achieve the above object, the technical scheme of the present invention is as follows:
a lithiated carbon point-based modified composite electrolyte comprising a polymer electrolyte and an interfacial layer on a surface of the polymer electrolyte, the interfacial layer comprising LiF; the polymer electrolyte comprises a high molecular polymer, lithium salt and lithiated carbon points; the lithiated carbon point is obtained by reacting acetaldehyde with a lithium precursor under alkaline conditions, wherein the lithium precursor comprises lithium bis (trifluoromethanesulfonyl) imide and/or lithium trifluorosulfonyl imide.
In some embodiments, the lithiated carbon point is 0.1 to 20% of the mass of the high molecular polymer.
In some embodiments, the lithiated carbon dots have an average particle size of 2 to 7nm.
In some embodiments, the high molecular polymer has a molecular weight of 200000 ～ 4000000g/mol.
In some embodiments, the high molecular polymer is selected from at least one of polyethylene oxide, polyacrylonitrile, polymethyl methacrylate, and polysiloxane.
In some embodiments, the lithium salt is selected from at least one of lithium perchlorate, lithium bis (trifluoromethanesulfonyl) imide, lithium trifluoromethanesulfonate, lithium bis (fluorosulfonyl) imide, lithium trifluoromethanesulfonate, lithium formate difluoroborate.
Another object of the present invention is to provide the method for preparing a composite electrolyte according to any one of the above embodiments, comprising the steps of:
s1, preparing lithiated carbon points: mixing the acetaldehyde and the lithium precursor, and reacting under alkaline conditions to obtain lithiated carbon points;
s2, adding the lithiated carbon point, the lithium salt and the high molecular polymer prepared in the step S1 into an organic solvent, uniformly mixing, pouring into a mold, and removing the solvent to obtain a polymer electrolyte;
s3, assembling the polymer electrolyte obtained in the step S2, the positive electrode and the lithium-containing metal negative electrode into an electrochemical energy storage device, and performing at least one charge-discharge cycle to obtain the composite electrolyte.
In the preparation method, the lithium symmetrical battery and the all-solid-state battery can be assembled, and the conditions of the charge and discharge cycle are normal voltages known in the art when the battery (or the capacitor) is charged and discharged, such as: when assembled into a lithium symmetrical battery, the current density is 0.05-0.5 mA/cm 2 Circulating the mixture; when the full battery is assembled, the cycle is carried out under the voltage of 2.5-4.3V; and are not described in detail herein.
In some embodiments, in step S1, specifically: mixing the acetaldehyde and the lithium precursor, adding 0.1-12 mol/L sodium hydroxide, and reacting for 2-72 h.
In some embodiments, in step S2, the solvent may be volatilized at room temperature and then dried under vacuum to completely remove the solvent.
It is a further object of the present invention to provide an electrochemical energy storage device comprising the composite electrolyte of any of the above embodiments.
In some embodiments, the electrochemical energy storage device is a lithium metal battery, a lithium air battery, a lithium carbon dioxide battery, or the like, having lithium-containing metal as the negative electrode.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the polymer and the lithiated carbon dots obtained by a specific method are mixed to prepare the composite electrolyte, and the composite electrolyte can form a LiF-rich interface layer on the surface of the electrolyte through in-situ chemical reaction with a lithium-containing metal negative electrode when in use, the LiF-rich interface layer plays a role in stabilizing the surface of the electrolyte, helps to quickly transfer ions, effectively solves the problem of dendrite generated by uneven lithium deposition caused by uneven charge, improves the cycling stability of the composite electrolyte, and further improves the cycle life and the service life of an electrochemical energy storage device.
In addition, the conductive polymer is added with lithiated carbon points which are used as a lithium conductor, so that the size of anions is large and difficult to move, free lithium ions can be dissociated, and the migration number of lithium ions of an electrolyte system is effectively improved. Meanwhile, the addition of the lithiated carbon point can destroy the regularity of the conductive polymer, improve the chain segment ion transmission efficiency and further improve the ion conductivity of the composite electrolyte.
Drawings
FIG. 1 is a transmission electron microscope image of lithiated carbon dots in example 1;
FIG. 2 is a polarization graph of a lithium symmetric battery of the composite electrolyte of example 1;
fig. 3 is XPS analysis of interface components after cycling of the lithium symmetric battery of the composite electrolyte in example 1.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit or scope of the invention, which is therefore not limited to the specific embodiments disclosed below.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
A preparation method of the composite electrolyte comprises the following steps:
s1, preparing lithiated carbon points: 4g of bis (trifluoromethane) sulfonyl imide lithium salt is added into 40ml of acetaldehyde solution, the mixture is stirred uniformly, 7.5g/L sodium hydroxide is added for reaction for 2 hours, and lithiated carbon points are obtained through dialysis and purification. The average size of lithiated carbon points is 2-5.2 nm through a transmission electron microscope test, and the test result is shown in figure 1;
s2, dispersing lithium perchlorate and the lithiated carbon point prepared in the step S1 and polyoxyethylene with the molecular weight of 2000000g/mol in an anhydrous acetonitrile solvent, stirring for 24 hours at room temperature, pouring the mixture on a die, volatilizing for 18 hours at room temperature, and then drying in vacuum to obtain a polymer electrolyte with the thickness of 90 mu m; wherein, the mole ratio of lithium perchlorate to oxyethylene chain segment in polyoxyethylene is 1:20, the mass of carbon points is 1% of the mass of polyoxyethylene;
s3, assembling the polymer electrolyte prepared in the step S2 into a lithium symmetrical battery, wherein the current density is 0.2mA/cm 2 And (3) carrying out 500 cycles of charge and discharge at 50 ℃ to obtain the composite electrolyte.
As shown in FIG. 2, the composite electrolyte obtained by the method of the invention has the lithium ion migration number of 0.60 and the ion conductivity of 1.0X10 -4 S/cm. The lithium symmetric battery did not generate lithium dendrites after 500 cycles. In addition, as shown in fig. 3, the composite electrolyte has a LiF-rich interface layer on the surface, and the interface is stable.
Example 2
A preparation method of the composite electrolyte comprises the following steps:
s1, preparing lithiated carbon points: embodiment as in example 1;
s2, dispersing the lithium bistrifluoro sulfonyl imide, the lithiated carbon point prepared in the step S1, the lithium bistrifluoro sulfonyl imide and polyoxyethylene with the molecular weight of 500000g/mol in an anhydrous acetonitrile solvent, stirring at room temperature for 24 hours, pouring the mixture on a mold, volatilizing at room temperature for 18 hours, and then drying in vacuum to obtain a polymer electrolyte; the polymer electrolyte thickness was 87 μm; wherein, the mole ratio of the lithium bistrifluorosulfonimide to the polyoxyethylene chain segment is 1:20, the mass of carbon points is 3% of the mass of polyoxyethylene;
s3, assembling the polymer electrolyte obtained in the step S2, a positive electrode and a lithium negative electrode into an all-solid-state battery, and performing at least one charge-discharge cycle under the voltage of 2.5-4.3V to obtain the composite electrolyte.
The composite electrolyte has a lithium ion migration number of 0.52 and an ion conductivity of 0.9X10 -4 S/cm。
Example 3
A preparation method of the composite electrolyte comprises the following steps:
s1, preparing lithiated carbon points: adding 4g of bis (trifluoromethane) sulfonyl imide lithium salt into 40mL of acetaldehyde solution, then adding 7.5g/L sodium hydroxide, reacting for 24h, and dialyzing and purifying to obtain lithiated carbon points;
s2, dissolving the lithiated carbon point obtained in the step S1, lithium perchlorate and polyoxyethylene with the molecular weight of 2000000g/mol in an anhydrous acetonitrile solvent, stirring at room temperature for 24 hours, pouring the mixture on a die, volatilizing at room temperature for 24 hours, and then drying in vacuum to obtain a polymer electrolyte; the polymer electrolyte has a thickness of 95 μm; wherein, the mole ratio of lithium perchlorate to oxyethylene chain segment in polyoxyethylene is 1:20, the mass of carbon points is 3% of the mass of polyoxyethylene;
s3, assembling the polymer electrolyte obtained in the step S2 into a lithium symmetrical battery, wherein the current density is 0.2mA/cm 2 And (3) carrying out a charge-discharge cycle at 50 ℃ to obtain the composite electrolyte.
The composite electrolyte obtained in the embodiment has the lithium migration number of 0.45 and the ion conductivity of 3.16X10 -5 S/cm。
Comparative example 1
A method of preparing a solid electrolyte comprising the steps of:
s1, adding polyoxyethylene with the molecular weight of 2000000g/mol and lithium perchlorate into an anhydrous acetonitrile solvent, stirring at room temperature for 24 hours, pouring the mixture on a mold, volatilizing at room temperature for 18 hours, and then drying in vacuum to obtain a solid electrolyte; the thickness of the solid electrolyte is 90 mu m, wherein the molar ratio of lithium perchlorate to oxyethylene chain segments in polyoxyethylene is 1:20, a step of;
s2, assembling the solid electrolyte obtained in the step S1 into a lithium symmetrical battery, wherein the current density is 0.2mA/cm 2 And carrying out 500 charge-discharge cycles at 50 ℃.
The solid electrolyte has an ionic conductivity of 6.67×10 -6 S/cm, the migration number of lithium ions is 0.21. The lithium symmetric battery produced lithium dendrites after 500 cycles, while the electrolyte surface did not contain LiF.
Comparative example 2
A solid state electrolyte, the method of making comprising the steps of:
s1, preparing lithiated carbon points: adding 1g of glucose and 40mL of ethanol into a reaction kettle respectively, completely sealing, and then placing the mixture into a muffle furnace to be heated to 160 ℃ for reaction for 12h; cooling to room temperature after the reaction is finished, adding the reaction product into a round-bottom flask, and removing ethanol by using a rotary evaporator; adding the obtained solid and lithium hydroxide into deionized water for lithiation reaction, and adjusting the pH value to be 8 to obtain a lithiated carbon point aqueous solution; adding the lithiated carbon point aqueous solution into a round-bottomed flask, and removing water by a rotary evaporator to obtain dried lithiated carbon point powder; wherein the average diameter of the lithiated carbon points is 3-8 nm;
s2, dispersing the lithiated carbon point, lithium perchlorate and polyoxyethylene with the molecular weight of 2000000g/mol prepared in the step S1 in anhydrous acetonitrile solution, stirring at room temperature for 24 hours, pouring the mixture on a die, volatilizing at room temperature for 18 hours, and then drying in vacuum to obtain a polymer electrolyte; the thickness of the composite electrolyte is 90 mu m; wherein, the mole ratio of lithium perchlorate to oxyethylene chain segment in polyoxyethylene is 1:20, the mass of the granulated carbon dots is 1% of the mass of polyoxyethylene;
s3, assembling the obtained polymer electrolyte into a lithium symmetrical battery, and carrying out 500 cycles of charge and discharge at the current density of 0.2mA/cm < 2 > and the temperature of 50 ℃ to obtain the solid electrolyte.
The solid electrolyte obtained in this comparative example was tested to have a lithium ion migration number of 0.65 and an ion conductivity of 0.92×10 -4 S/cm. The solid electrolyte was subjected to interface analysis, and no LiF interface layer was detected.
In summary, the composite electrolyte provided by the invention can greatly improve the migration number and the ion conductivity of lithium ions while ensuring the cycling stability of the electrolyte.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. A lithiated carbon point-based modified composite electrolyte comprising a polymer electrolyte and an interfacial layer on a surface of the polymer electrolyte, the interfacial layer comprising LiF; the polymer electrolyte comprises a high molecular polymer, lithium salt and lithiated carbon points; the lithiated carbon point is obtained by reacting acetaldehyde with a lithium precursor under alkaline conditions, wherein the lithium precursor comprises lithium bis (trifluoromethanesulfonyl) imide and/or lithium trifluorosulfonyl imide.
2. The lithiated carbon dot modified composite electrolyte of claim 1, wherein the mass of the lithiated carbon dot is 0.1 to 20% of the mass of the high molecular polymer.
3. The lithiated carbon point modified composite electrolyte of claim 1, wherein the high molecular polymer has a molecular weight of 200000 ～ 4000000g/mol.
4. The lithiated carbon point-modified composite electrolyte of claim 1, wherein the high molecular polymer is selected from at least one of polyethylene oxide, polyacrylonitrile, polymethyl methacrylate, and polysiloxane.
5. The lithiated carbon point-modified composite electrolyte of claim 1, wherein the lithium salt is selected from at least one of lithium perchlorate, lithium bis (trifluoromethanesulfonyl) imide, lithium trifluoromethanesulfonate, lithium bis (fluorosulfonyl) imide, lithium trifluoromethanesulfonate, lithium formate difluoroborate.
6. The lithiated carbon dot modified composite electrolyte of claim 1, wherein the lithiated carbon dot has an average particle diameter of from 2 to 7nm.
7. The method for producing a lithiated carbon point-modified composite electrolyte in accordance with any one of claims 1 to 6, comprising the steps of:
s1, preparing lithiated carbon points: mixing the acetaldehyde and the lithium precursor, and reacting under alkaline conditions to obtain lithiated carbon points;
s2, adding the lithiated carbon point, the lithium salt and the high molecular polymer prepared in the step S1 into an organic solvent, uniformly mixing, pouring into a mold, and removing the solvent to obtain a polymer electrolyte;
s3, assembling the polymer electrolyte obtained in the step S2, the positive electrode and the lithium-containing metal negative electrode into an electrochemical energy storage device, and performing at least one charge-discharge cycle to obtain the composite electrolyte.
8. The method for preparing a lithiated carbon point modified composite electrolyte in accordance with claim 7, wherein in step S1, specifically: mixing the acetaldehyde and the lithium precursor, adding 0.1-12 mol/L sodium hydroxide, and reacting for 2-72 h.
9. The method for producing a lithiated carbon point-modified composite electrolyte of claim 7, wherein in step S2, the solvent is volatilized under vacuum.
10. An electrochemical energy storage device comprising the lithiated carbon dot modified composite electrolyte of any one of claims 1 to 6.
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