CN113161619A - Weak-polarity system electrolyte and application thereof - Google Patents
Weak-polarity system electrolyte and application thereof Download PDFInfo
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- CN113161619A CN113161619A CN202110474267.4A CN202110474267A CN113161619A CN 113161619 A CN113161619 A CN 113161619A CN 202110474267 A CN202110474267 A CN 202110474267A CN 113161619 A CN113161619 A CN 113161619A
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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
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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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
- 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
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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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
- H01M2300/0025—Organic 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the technical field of electrolyte, in particular to weak-polarity system electrolyte and application thereof. The invention provides a weak-polarity system electrolyte, which comprises a silicate compound, an inert shielding agent and a non-aqueous electrolyte lithium salt. The weak-polarity system electrolyte can improve the damage of the volume change of the silicon-based negative electrode to the interface layer in the charging and discharging processes, and improve the cycle stability of the silicon-based negative electrode lithium ion battery.
Description
Technical Field
The invention relates to the technical field of electrolyte, in particular to weak-polarity system electrolyte and application thereof.
Background
Silicon has received much attention as a promising negative electrode material for next-generation lithium ion batteries due to its high theoretical capacity and breadth. However, since the volume change of silicon is too large (more than 300%) during the lithium ion intercalation/deintercalation process, the problems of breakage, pulverization, etc. of the silicon negative electrode are caused, which hinders the practical application of the silicon negative electrode. During the cyclic charge and discharge of lithium batteries, the electrolyte solution starts thereinThe lithium ion battery has the advantages that the lithium ion battery has an extremely important function, and due to the existence of the electrolyte solution, when the battery is subjected to lithium ion intercalation and deintercalation reaction, the generated lithium ions can flow between the positive electrode and the negative electrode through the electrolyte solution, so that the electrolyte solution in the lithium ion battery is connected with the positive electrode and the negative electrode like a bridge, and the performance of the battery can be obviously improved only by searching for a more appropriate electrolyte material. And because silicon has huge volume expansion from the beginning, how to select a more appropriate electrolyte to form a stable SEI film on the surface of the negative electrode is the first problem to be solved by the electrolyte of the silicon negative electrode. It is well known in the art that a conventional electrolyte for silicon-based negative electrodes is LiPF6Carbonate-based electrolytes, in which an amount of fluoroethylene carbonate (FEC) is contained as an additive or a co-solvent (5 to 10 wt% of the electrolyte), the Solid Electrolyte Interphase (SEI) formed on the surface of the silicon-based negative electrode by the carbonate-based electrolytes in the above conventional electrolytes is unstable and cannot withstand large volume changes of silicon during cycling. Although the introduction of FEC carbonate electrolyte may improve the cycling performance of silicon cathodes, an increase in the amount of FEC may lead to an increase in gassing in the cell, which in turn leads to an increase in impedance, capacity fade and safety issues.
Disclosure of Invention
The invention aims to provide a weak-polarity system electrolyte and application thereof, wherein the weak-polarity system electrolyte can improve the damage of volume change of a silicon-based negative electrode to an interface layer in the charging and discharging processes and improve the cycle stability of a silicon-based negative electrode lithium ion battery.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a weak-polarity system electrolyte, which comprises a silicate compound, an inert shielding agent and a non-aqueous electrolyte lithium salt;
the silicate ester compound comprises a compound with a structure shown in a formula I:
wherein n is an integer of 0 to 3.
Preferably, the silicate-based compound comprises tetramethyl silicate, tetraethyl silicate or tetrabutyl silicate.
Preferably, the inert shielding agent comprises one or more of symmetric oxygen-free alkane, symmetric oxygen-free silane, aromatic hydrocarbon and carbon tetrachloride.
Preferably, the symmetric oxygen-free alkane comprises a symmetric cycloalkane;
the symmetrical oxygen-free silane comprises tetramethylsilane and/or hexamethyldisilane;
the aromatic hydrocarbon includes benzene.
Preferably, the non-aqueous electrolyte lithium salt includes one or more of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium perchlorate, lithium bis (trifluoromethylsulfonyl) imide and lithium bis (sulfonyl fluoride) imide.
Preferably, the volume ratio of the silicate compound to the inert shielding agent is (1-3): 1.
preferably, the concentration of the non-aqueous electrolyte lithium salt in the weak polar system electrolyte is 0.1-4 mol/L.
The invention also provides the application of the weak-polarity system electrolyte in the silicon-based negative electrode of the lithium ion battery.
The invention provides a weak-polarity system electrolyte, which comprises a silicate compound, an inert shielding agent and a non-aqueous electrolyte lithium salt;
the silicate ester compound comprises a compound with a structure shown in a formula I:
wherein n is an integer of 0 to 3.
Compared with the prior art, the technical scheme provided by the invention has the following excellent effects:
1) according to the invention, silicate compounds (weak-polarity solvents) are used as solvents of the electrolyte, and an electrolyte system with low cost, low toxicity, good wettability and excellent performance is obtained by compounding the silicate compounds and the non-polar inert shielding agent according to the principle of similarity and intermiscibility;
2) according to the invention, the silicate ester compound is used as a special coexisting structure of a solvent and a lithium salt (the special coexisting structure is in the silicate ester compound, when the lithium salt is dissolved in the solvent, the lithium salt cannot be completely dissociated, the large logarithm exists in the form of an ion pair, and the binding energy of lithium ions and anions is greater than the coordination binding energy of the lithium ions and the solvent), so that the lithium salt is enough to be used as a leading substance for reductive decomposition in a circulation process under the condition of meeting the concentration of the lithium salt, the effect of dissolving the high-concentration lithium salt in the polar solvent is achieved, and the inert shielding agent does not have solvation with the lithium salt, and the poor decomposition of the solvent can be effectively inhibited;
3) in the process of charging and discharging the electrolyte, the nonaqueous electrolyte lithium salt is a reducing substance, and an SEI film (LiF, Li) rich in inorganic products can be generated3N, etc.). Meanwhile, silicate compounds are reduced in a small part at a low potential to form Si-O-Si crosslinking with the silicon surface, so that an organic-inorganic composite interface layer which takes inorganic matters as a main component and takes Si-O-Si as a framework is formed in the reduction process, the damage of the volume change of a silicon-based negative electrode to the interface layer in the charging and discharging process is further improved, and the overall cycling stability of the battery is improved;
4) the silicate compound is extremely sensitive to water bath acid, silicon dioxide is generated when the silicate compound is contacted with water, the silicate compound serving as electrolyte in a closed system of the battery can also prevent the side effect of trace (PPM) water and acid on an electrode structure, and due to the characteristic, a solvent is easily and highly purified in the practical application process, and a high-purity reagent is in the electrolyte, so that the electrochemical window can be widened (the electrochemical stability of the solvent is improved).
Drawings
FIG. 1 is a graph comparing the cycle capacity retention rates of half-cells prepared from the electrolytes described in example 1 and comparative examples 1 to 3;
FIG. 2 is a graph showing the variation of coulombic efficiency with cycle number of half cells prepared from the electrolytes described in example 1 and comparative examples 1 to 3;
FIG. 3 is an XPS (X-ray diffraction) chart of the surface of a silicon-based negative electrode of a half cell prepared from the electrolyte solution described in example 1 and comparative examples 1-2 after the half cell tests cyclic voltammetry for 3 circles at an electrochemical workstation;
FIG. 4 is a SEM image of a cross section of a silicon negative electrode in a half cell prepared by the electrolyte solutions of example 1 and comparative examples 1-2 after circulating for 50 cycles;
FIG. 5 is a surface SEM image of silicon cathodes in half-cells prepared from the electrolytes described in example 1 and comparative examples 1-2 after 50 cycles.
Detailed Description
The invention provides a weak-polarity system electrolyte, which comprises a silicate compound, an inert shielding agent and a non-aqueous electrolyte lithium salt;
the silicate ester compound comprises a compound with a structure shown in a formula I:
wherein n is an integer of 0 to 3.
In the present invention, the silicate-based compound preferably includes tetramethyl silicate, tetraethyl silicate, or tetrabutyl silicate.
In the invention, the inert shielding agent comprises one or more of symmetrical oxygen-free alkane, symmetrical oxygen-free silane, aromatic hydrocarbon and carbon tetrachloride; the symmetric oxygen-free alkane preferably comprises a symmetric cycloalkane; the symmetrical cycloalkanes preferably comprise cyclohexane and/or cyclooctane; the symmetrical oxygen-free silane preferably comprises tetramethylsilane and/or hexamethyldisilane; the aromatic hydrocarbon preferably comprises benzene. When the inert shielding agent is more than two of the specific choices, the proportion of the specific substances is not limited in any way, and the specific substances can be mixed according to any proportion. In the invention, the inert shielding agent is selected from symmetrical oxygen-free silane, symmetrical oxygen-free alkane, aromatic hydrocarbon or carbon tetrachloride and the like which do not generate solvation with lithium salt, so that the dosage of the lithium salt in the electrolyte can be further reduced, and the cost is reduced.
In the present invention, the non-aqueous electrolyte lithium salt includes one or more of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium perchlorate, lithium bis (trifluoromethylsulfonyl) imide and lithium bis (sulfonyl fluoride) imide; when the nonaqueous electrolyte lithium salt is two or more selected from the above specific choices, the present invention does not have any particular limitation on the compounding ratio of the specific materials, and the specific materials may be mixed in any compounding ratio.
In the invention, the volume ratio of the silicate compound to the inert shielding agent is preferably (1-3): 1, more preferably (1.5 to 2.5): 1, most preferably 2: 1.
In the invention, the concentration of the non-aqueous electrolyte lithium salt in the weak polar system electrolyte is preferably 0.1-4 mol/L, more preferably 0.65-1.5 mol/L, and most preferably 0.8-1.2 mol/L.
In the present invention, the preparation method of the weak polar system electrolyte is preferably: mixing a silicate compound and an inert shielding agent to obtain a mixed solvent; and mixing the non-aqueous electrolyte lithium salt with the mixed solvent, and stirring the mixture uniformly to obtain the weak-polarity electrolyte. The mixing and stirring process of the present invention is not particularly limited, and may be carried out by a process known to those skilled in the art.
In the present invention, the preparation process is preferably carried out in a glove box having a water content of less than 0.5ppm and an oxygen content of less than 0.5 ppm.
The invention also provides the application of the weak-polarity system electrolyte in the silicon-based negative electrode of the lithium ion battery. The method of the present invention is not particularly limited, and the method may be performed by a method known to those skilled in the art.
The weakly polar system electrolyte and the application thereof provided by the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
In a glove box with water content lower than 0.5ppm and oxygen content lower than 0.5ppm, preparing a weak-polarity system electrolyte:
mixing 10mL of tetraethyl silicate and 10mL of cyclohexane according to the volume ratio of 1:1 to obtain a mixed solvent;
0.016mol of lithium bis (sulfonyl fluoride) imide (LiFeSi) is mixed with 20mL of mixed solvent and stirred uniformly to obtain the weak polar system electrolyte with the concentration of LiFeSi being 0.8 mol/L.
Example 2
In a glove box with water content lower than 0.5ppm and oxygen content lower than 0.5ppm, preparing a weak-polarity system electrolyte:
mixing 20mL of tetraethyl silicate and 10mL of cyclohexane according to the volume ratio of 2:1 to obtain a mixed solvent;
0.036mol of lithium bis (sulfonyl fluoride) imide (LiFSI) is mixed with 30mL of mixed solvent and stirred uniformly to obtain the weak polar system electrolyte with the concentration of LiFSI of 1.2 mol/L.
Example 3
In a glove box with water content lower than 0.5ppm and oxygen content lower than 0.5ppm, preparing a weak-polarity system electrolyte:
mixing 30mL of tetraethyl silicate and 10mL of cyclohexane according to the volume ratio of 3:1 to obtain a mixed solvent;
0.08mol of lithium bis (sulfonyl fluoride) imide (LiFSI) is mixed with 40mL of mixed solvent and stirred uniformly to obtain the weak polar system electrolyte with the concentration of LiFSI of 2 mol/L.
Example 4
In a glove box with water content lower than 0.5ppm and oxygen content lower than 0.5ppm, preparing a weak-polarity system electrolyte:
mixing 10mL of tetraethyl silicate and 10mL of hexamethyldisilane according to the volume ratio of 1:1 to obtain a mixed solvent;
0.013mol of lithium bis (sulfonyl fluoride) imide (LiFSI) is mixed with 20mL of mixed solvent and stirred uniformly to obtain the weak polar system electrolyte with the LiFSI concentration of 0.65 mol/L.
Comparative example 1
In a glove box with water content lower than 0.5ppm and oxygen content lower than 0.5ppm, preparing a weak-polarity system electrolyte:
mixing 10mL of EC (ethylene carbonate), 10mL of DEC (diethyl carbonate) and 10mL of DMC (dimethyl carbonate) according to a volume ratio of 1:1:1 to obtain a mixed solvent;
0.03mol of LiPF6Mixing with 30mL of a mixed solvent, adding 3.5g of fluoroethylene carbonate (FEC) and 0.7g of Vinylene Carbonate (VC), and stirring uniformly to obtain LiPF6The concentration of (3) is 1.0 mol/L.
Comparative example 2
In a glove box with water content lower than 0.5ppm and oxygen content lower than 0.5ppm, preparing a weak-polarity system electrolyte:
mixing 10mL of EC (ethylene carbonate), 10mL of DEC (diethyl carbonate) and 10mL of DMC (dimethyl carbonate) according to a volume ratio of 1:1:1 to obtain a mixed solvent;
0.03mol of LiPF6Mixing with 30mL of mixed solvent to obtain LiPF6The concentration of (3) is 1.0 mol/L.
Comparative example 3
In a glove box with water content lower than 0.5ppm and oxygen content lower than 0.5ppm, preparing a weak-polarity system electrolyte:
0.016mol of LiFeSi is mixed with 20mL of tetraethyl silicate, and the mixture is uniformly stirred to obtain an electrolyte with the concentration of LiFeSi of 0.8 mol/L.
Test example
Preparing a silicon cathode of the lithium ion battery:
mixing and grinding 0.6g of commercial nano silicon particles (active substances), 0.2g of carbon black (conductive agent) and 5g of LiPAA aqueous solution (mass concentration is 4%, and binder), placing the mixture in a corundum ball milling tank, continuously adding 5mL of deionized water, and carrying out ball milling at the rotating speed of 400rpm for 12 hours to obtain mixed slurry;
uniformly coating the mixed slurry on a copper foil by using a coating machine, completely drying at 40 ℃, then drying in vacuum for 8-12 h at 100 ℃, and cutting to obtain the silicon cathode of the lithium ion battery;
in a glove box with water and oxygen less than 0.01ppm, lithium sheets are used as a counter electrode and a reference electrode, a silicon cathode of the lithium ion battery is used as a working electrode, Celgard (polypropylene, pp) is used as a diaphragm, the electrolytes described in examples 1-4 and comparative examples 1-3 are respectively used as electrolytes, half batteries are prepared, the dosage of the electrolyte in each half battery is 100 muL, after the preparation is finished, the half batteries are stood for 10 hours, and then a half battery electrochemical cycle test is carried out on a Neware CT-4000 battery tester in an environmental chamber at 25 ℃,
1) the test conditions were: the voltage window is 0.01-1.2V, and the current density of constant current charging and discharging is 420 mA-g-1. The test results are shown in fig. 1-2 and fig. 4-5, wherein fig. 1 is a comparison graph of the cycle capacity retention rate of the half-cell prepared by the electrolyte described in example 1 and comparative examples 1-3, and as can be seen from fig. 1, after 100 cycles, the half-cell prepared by the electrolyte described in the invention has more stable cycle stability, and after 100 cycles, the capacity retention rate is the highest;
the cycle capacity retention rate of the half-cell prepared by the electrolyte described in examples 1 to 4 and comparative examples 1 to 3 after 100 cycles is shown in table 1:
TABLE 1 Cyclic Capacity Retention ratio of half-cells prepared from the electrolytes described in examples 1 to 4 and comparative examples 1 to 3 after 100 cycles
As can be seen from Table 1, the cycle retention rates of the half-cells prepared in examples 1 to 4 are all superior to those of comparative examples 1 to 3.
FIG. 2 is a graph showing the variation of coulombic efficiency with cycle number of half cells prepared from the electrolytes described in example 1 and comparative examples 1 to 3; as can be seen from fig. 2, the half-cell prepared by the electrolyte of the present invention has higher circulating coulombic efficiency;
FIG. 4 is a SEM image of the cross section of a silicon negative electrode in a half cell prepared by the electrolyte solutions of example 1 and comparative examples 1-2 after 50 cycles, and it can be seen from FIG. 4 that in example 1, compared with comparative examples 1-2, the thickness of the electrode slice cross section is the smallest after 50 cycles, i.e. the volume expansion of the silicon negative electrode is most effectively inhibited;
fig. 5 is a surface SEM image of a silicon negative electrode in a half-cell prepared by the electrolyte solutions described in example 1 and comparative examples 1 to 2 after 50 cycles, and as can be seen from fig. 5, in example 1, compared with comparative examples 1 to 2, the surface of an electrode sheet is relatively flat after 50 cycles of cycles, which indicates that expansion of the silicon-based negative electrode has a relatively small influence on the integrity of the electrode structure.
2) The half-cells prepared from the electrolytes described in example 1 and comparative examples 1-2 were tested for cyclic voltammetry for 3 cycles in an electrochemical workstation under the following test conditions: the test temperature was 25 ℃ and the scan rate was 0.2mV s-1The scanning voltage range is: 0.01V-2.5V; the XPS test of the silicon-based negative electrode surface after the test is performed, and the test results are shown in fig. 3, where (a) is comparative example 1, (b) is comparative example 2, and (c) is example 1, and as can be seen from fig. 3, the large component distribution of the SEI film formed on the silicon negative electrode surface during the charge and discharge processes is: comparative example 1 has a fluorine atom content of 3.9%, comparative example 2 has a fluorine atom content of 1.5%, and example 1 has a fluorine atom content of 9.7%; therefore, the embodiment 1 has more inorganic substances, so that the surface of the silicon negative electrode derives the SEI film rich in LiF, compared with the SEI film rich in organic substances, the SEI film rich in LiF has higher strength, and the composite interface layer taking the inorganic substances as the leading part is more beneficial to relieving the damage of the volume expansion of the silicon negative electrode to the SEI film of the silicon negative electrode in the charging and discharging processes.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The weak-polarity system electrolyte is characterized by comprising a silicate compound, an inert shielding agent and a non-aqueous electrolyte lithium salt;
the silicate ester compound comprises a compound with a structure shown in a formula I:
wherein n is an integer of 0 to 3.
2. The weak polar system electrolyte of claim 1, wherein the silicate compound comprises tetramethyl silicate, tetraethyl silicate, or tetrabutyl silicate.
3. The weak polar system electrolyte of claim 1 wherein the inert shielding agent comprises one or more of a symmetric oxygen-free alkane, a symmetric oxygen-free silane, an aromatic hydrocarbon, and carbon tetrachloride.
4. The weak polar system electrolyte of claim 3 wherein the symmetric oxygen-free alkane comprises symmetric cycloalkane;
the symmetrical oxygen-free silane comprises tetramethylsilane and/or hexamethyldisilane;
the aromatic hydrocarbon includes benzene.
5. The weak polar system electrolyte according to claim 1, wherein the non-aqueous electrolyte lithium salt includes one or more of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium perchlorate, lithium bis (trifluoromethylsulfonyl) imide and lithium bis (sulfonyl fluoride) imide.
6. The weak-polarity-system electrolyte according to claim 1, wherein the volume ratio of the silicate compound to the inert shielding agent is (1-3): 1.
7. the weak polar system electrolyte of claim 1 or 6, wherein the concentration of the non-aqueous electrolyte lithium salt in the weak polar system electrolyte is 0.1 to 4 mol/L.
8. The application of the weak-polarity-system electrolyte as claimed in any one of claims 1 to 7 in a silicon-based negative electrode of a lithium ion battery.
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