CN114695965A - Interface wetting agent for halide solid electrolyte - Google Patents
Interface wetting agent for halide solid electrolyte Download PDFInfo
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- 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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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to an interface wetting agent for a halide solid electrolyte. The raw materials for preparing the interfacial wetting agent comprise a solvent and lithium salt, wherein the solvent is one or two of n-butyl ether or isobutyl ether; the lithium salt includes lithium bistrifluoromethanesulfonylimide. The interface wetting agent provided by the invention has the advantages of wide electrochemical window, stability with halide solid electrolyte and the like. When the composite material is used in a solid-state battery, the compactness of an electrode can be improved, the conductivity between solid-solid interfaces can be improved, and the solid-solid interface impedance can be reduced, so that the performance of the solid-state battery can be improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to an interface wetting agent for a halide solid electrolyte.
Background
The solid-state battery has the advantages of high safety performance, high energy density (expected to reach 300-400 Wh/kg or even higher), long cycle life (expected to avoid the problem that SEI (solid electrolyte interphase) films and lithium dendrites formed in the charging and discharging processes of liquid electrolytes pierce diaphragms), wide working temperature range (good needling and high-temperature stability), high production efficiency, good flexibility and the like, so that the solid-state battery becomes one of the mainstream directions of future battery development.
The development of solid electrolytes is one of the most critical steps for solid-state batteries. Currently, most studied solid electrolytes mainly include polymers, oxides, sulfides, halides, and the like, wherein the halides have high ionic conductivity, stable chemical/electrochemical stability, good plasticity, and a high oxidation stability potential (4.2V) (adv. mater.2018,1803075), and have good compatibility with lithium cobaltate positive electrode materials, ternary positive electrode materials, and lithium-rich manganese-based positive electrode materials. Therefore, the halide solid electrolyte becomes the most potential electrolyte for application in solid batteries.
The interfacial problem between the solid electrolyte and the electrodes is a major factor limiting its commercial application on a large scale. In contrast to conventional liquid batteries, interfaces between the positive electrode-electrolyte interface, the negative electrode-electrolyte interface, and the inorganic particles occur in solid-state batteries, and the migration of lithium ions at these interfaces determines the overall conductivity of the solid-state electrolyte and the overall performance of the battery (Joule 2, 1-25, October 17,2018). The interfacial wetting agent in the prior art has the problem of low oxidation potential after being applied to halide solid-state electrolysis, and cannot be effectively applied. Disclosure of Invention
Aiming at the problem that the effect of the interface wetting agent of the halide solid electrolyte in the prior art is not ideal, the invention provides the interface wetting agent specially used for the halide solid electrolyte. The raw materials for preparing the wetting agent comprise a solvent and lithium salt, wherein the solvent is one or two of n-butyl ether or isobutyl ether; the lithium salt includes lithium bistrifluoromethanesulfonylimide.
The invention discovers that the interface wetting agent prepared by using lithium bistrifluoromethanesulfonylimide (LiTFSI) as a lithium salt and n-butyl ether or isobutyl ether as a solvent has the advantage of high oxidation potential and stable performance after being mixed with a halide solid electrolyte in the process of being applied to the halide solid electrolyte.
Preferably, the concentration of the lithium salt in the solvent is 2-3 mol/L.
Preferably, the lithium salt further comprises lithium bis (fluorosulfonyl) imide (LiFSI).
Preferably, the lithium salt is a mixture of lithium bis (trifluoromethane sulfonyl) imide and lithium bis (fluorosulfonyl) imide, and the molar percentage of the lithium bis (trifluoromethane sulfonyl) imide is greater than or equal to 50%. After the lithium bis (fluorosulfonyl) imide is added, the electrochemical window of the material is reduced to a certain extent, but within the addition amount, the electrochemical window is not obviously affected, and the subsequent application range can be expanded.
Preferably, the chemical composition formula of the halide solid electrolyte is LiaMbXcWherein M comprises at least one selected from metallic elements and semimetallic elements except Li, and X comprises at least one selected from F, Cl, Br, I.
The invention also provides a preparation method of the interfacial wetting agent, which comprises the following steps:
in a glove box filled with argon, the lithium salt was weighed and added to the solution until completely dissolved.
The invention also protects a lithium ion battery or a lithium battery of the interface wetting agent.
Preferably, the lithium ion battery or the lithium battery is a halide solid electrolyte-high nickel positive electrode material system or a lithium-rich manganese-based high-voltage positive electrode material system.
The invention has the following beneficial effects:
the interface wetting agent provided by the invention has the advantages of wide electrochemical window, stability with halide solid electrolyte and the like. When the composite material is used in a solid-state battery, the compactness of an electrode can be improved, the conductivity between solid-solid interfaces can be improved, and the solid-solid interface impedance can be reduced, so that the performance of the solid-state battery can be improved.
Drawings
FIG. 1 is an XRD pattern of a halide solid electrolyte after being mixed with an interfacial wetting agent and left standing for 1 d;
FIG. 2 is the first charge and discharge curve for 0.1C without the addition of the interfacial wetting agent cell (Li-In/Li3InCl6+ Li10GeP2S12/LiNiCoMn + Li3InCl6) and with the addition of the interfacial wetting agent cell (Li-In/Li3InCl6+ Li10GeP2S12/LiNiCoMn + Li3InCl6+ interfacial wetting agent);
FIG. 3 0.1C cycle curves without the addition of the interfacial wetting agent cell (Li-In/Li3InCl6+ Li10GeP2S12/LiNiCoMn + Li3InCl6) and with the addition of the interfacial wetting agent cell (Li-In/Li3InCl6+ Li10GeP2S12/LiNiCoMn + Li3InCl6+ interfacial wetting agent);
FIG. 4 impedance contrast curves after cycling without the addition of the interfacial wetting agent cell (Li-In/Li3InCl6+ Li10GeP2S12/LiNiCoMn + Li3InCl6) and with the addition of the interfacial wetting agent cell (Li-In/Li3InCl6+ Li10GeP2S12/LiNiCoMn + Li3InCl6+ interfacial wetting agent);
Detailed Description
The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
The following examples are intended only to further illustrate the present invention and should not be construed as limiting the invention. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention.
Unless otherwise specified, the test reagents and materials used in the examples of the present invention are commercially available.
Unless otherwise specified, the technical means used in the examples of the present invention are conventional means well known to those skilled in the art.
Example 1
According to the proportion of 0.02mol of LiTFSI and 10mL of n-butyl ether, weighing LiTFSI in a jacket box filled with argon (with water content of 1ppm and oxygen of 1ppm), then adding the n-butyl ether into the LiTFSI, stirring for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; testing the conductivity of the interfacial wetting agent using a conductivity tester; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Example 2
Weighing LiTFSI according to the proportion of 0.026mol of LiTFSI and 10mL of n-butyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the n-butyl ether into the LiTFSI, stirring the mixture for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; testing the conductivity of the interfacial wetting agent using a conductivity tester; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Example 3
Weighing LiTFSI according to the proportion of 0.030mol of LiTFSI and 10mL of n-butyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the n-butyl ether into the LiTFSI, stirring the mixture for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; testing the conductivity of the interfacial wetting agent using a conductivity tester; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Example 4
Weighing LiTFSI according to the proportion of 0.02mol of LiTFSI and 10mL of isobutyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), then adding n-butyl ether into the LiTFSI, stirring for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; testing the conductivity of the interfacial wetting agent using a conductivity tester; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Example 5
According to 0.02mol LiFSI/LiFSI, wherein the molar ratio of LiFSI to LiFSI is 1: 1. proportioning with 10mL of n-butyl ether, weighing LiFSI in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the n-butyl ether into the LiFSI, stirring for 30 minutes, and completely dissolving lithium salt to obtain an interface wetting agent; testing the conductivity of the interfacial wetting agent using a conductivity tester; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Example 6
The interfacial wetting agent of example 1 was used for TG-DSC test to test thermal stability.
Example 7
Mixing Li3InCl6Soaking in the interface wetting agent prepared in example 2 for 1 day, taking out part of the solid electrolyte, drying in a vacuum drying oven, and testing XRD and ionic conductivity.
Example 8
In a glove box filled with argon (moisture 1ppm, oxygen 1ppm), ordinary LiNiCoMo was used as a positive electrode material. Taking the positive electrode material: li3InCl6: conductive agent: the interfacial wetting agent electrode additive material is 59.85: 25.65: 4.5: 10 (mass ratio) are fully mixed, and the mixing process is carried out in a glove box. Using metal thin lithium-indium alloy as negative electrode and Li3InCl6Is an electrolyte material. Taking 70 mg of Li3InCl6The cross-sectional area of the insert was 0.785cm2The mold battery inner container (2) was pressed at a pressure of 150 MPa, and 30 mg of Li was added to the electrolyte layer side10GeP2S12After being uniformly paved, the mixture is pressed for the second time under the pressure of 150 MPa, and an electrolyte layer is obtained; in Li3InCl6Adding 12 mg of anode powder, uniformly spreading, tabletting under 350 MPa, and laminating the anode layer and the electrolyte; in Li10GeP2S12Putting Li-In into one sideThe sheet serves as a negative electrode layer. After the whole process is finished, the inner container is placed into the battery of the die, and the screw is tightly pressed and screwed for sealing. After sealing, the Li-In/Li In all solid state can be obtained3InCl6+Li10GeP2S12/LiNiCoMn+Li3InCl6+ C + interfacial wetting agent secondary battery.
Comparative example 1
Weighing LiTFSI according to the proportion of 0.02mol of LiTFSI and 10mL of diethyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the diethyl ether into the LiTFSI, stirring the mixture for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; TG-DSC tests were carried out.
Comparative example 2
Weighing LiTFSI according to the proportion of 0.02mol of LiTFSI and 10mL of isopropyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the isopropyl ether into the LiTFSI, stirring the mixture for 30 minutes, and completely dissolving lithium salt to obtain the interfacial wetting agent; TG-DSC tests were carried out.
Comparative example 3
Weighing the LiTFSI according to the proportion of 0.02mol of LiTFSI and 10mL of n-amyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the n-amyl ether into the LiTFSI, stirring for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; the interfacial wetting agent was tested for conductivity using a conductivity tester.
Comparative example 4
Weighing the LiTFSI according to the proportion of 0.02mol of LiTFSI and 10mL of n-hexyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the n-hexyl ether into the LiTFSI, stirring for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; the interfacial wetting agent was tested for conductivity using a conductivity tester.
Comparative example 5
Weighing LiTFSI in a hand box filled with argon according to the proportion of 0.02mol of LiFSI and 10mL of isopropyl ether (water content is 1ppm, oxygen content is 1ppm), adding the isopropyl ether into the LiTFSI, stirring the mixture for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Comparative example 6
Weighing LiTFSI according to the proportion of 0.02mol LiFSI to 10mL n-butyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the n-butyl ether into the LiTFSI, stirring the mixture for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Comparative example 7
Weighing LiTFSI in a glove box filled with argon according to the proportion of 0.02mol of LiFSI to 10mL of n-amyl ether (water content is 1ppm, oxygen is 1ppm), adding the n-amyl ether into the LiTFSI, stirring for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Comparative example 8
Weighing LiTFSI according to the proportion of 0.02mol LiFSI to 10mL n-hexyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the n-hexyl ether into the LiTFSI, stirring for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Comparative example 9
According to 0.02mol of LiPF6Blending with 10mL of n-butyl ether, LiPF was weighed in a glove box filled with argon (moisture 1ppm, oxygen 1ppm)6Then adding n-butyl ether, heating and stirring at 60 ℃ for 2 hours until the lithium salt is not completely dissolved to obtain an interfacial wetting agent; the interfacial wetting agent was tested for conductivity using a conductivity tester.
Comparative example 10
Weighing LiBOB in a proportion of 0.02mol of LiBOB to 10mL of n-butyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the n-butyl ether into the LiBOB, heating and stirring the mixture at the temperature of 60 ℃ for 2 hours until lithium salt is not completely dissolved to obtain an interfacial wetting agent; the interfacial wetting agent was tested for conductivity using a conductivity tester.
Comparative example 11
Weighing LiDFOB in a glove box filled with argon according to the proportion of 0.02mol of LiDFOB to 10mL of n-butyl ether (water content is 1ppm and oxygen is 1ppm), adding the n-butyl ether into the LiDFOB, heating and stirring the mixture at the temperature of 60 ℃ for 2 hours until lithium salt is not completely dissolved to obtain an interfacial wetting agent; the interfacial wetting agent was tested for conductivity using a conductivity tester.
Comparative example 12
Weighing LiTFSI according to the proportion of 0.015mol of LiTFSI and 10mL of n-butyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), then adding the n-butyl ether into the LiTFSI, stirring the mixture for 30 minutes, and completely dissolving lithium salt to obtain the interface wetting agent; testing the conductivity of the interfacial wetting agent using a conductivity tester; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Comparative example 13
Weighing LiTFSI according to the proportion of 0.036mol of LiTFSI and 10mL of n-butyl ether in a glove box filled with argon (with the water content of 1ppm and the oxygen content of 1ppm), adding the n-butyl ether into the LiTFSI, stirring the mixture for 30 minutes, and completely dissolving lithium salt to obtain the interfacial wetting agent; testing the conductivity of the interfacial wetting agent using a conductivity tester; the Li-stainless steel button cell was assembled and the interfacial wetting agent electrochemical window was tested.
Comparative example 14
In a glove box filled with argon (moisture 1ppm, oxygen 1ppm), normal LiNiCoMn was used as a positive electrode material. Taking the positive electrode material: li3InCl6: the conductive agent is 66.5: 28.5: 5 (mass ratio) and the mixing process is carried out in a glove box. Using metal thin lithium-indium alloy as negative electrode and Li3InCl6Is an electrolyte material. Taking 70 mg of Li3InCl6The cross-sectional area of the insert was 0.785cm2The mold battery inner container (2) was pressed into a tablet at a pressure of 150 MPa, and 30 mg of Li was added to one side10GeP2S12After being uniformly paved, the mixture is pressed for the second time under the pressure of 150 MPa, and an electrolyte layer is obtained; in Li3InCl6Adding 12 mg of anode powder, uniformly spreading, tabletting under 350 MPa, and laminating the anode layer and the electrolyte; in Li10GeP2S12One side ofAnd putting a Li-In sheet as a negative electrode layer. After the whole process is finished, the inner container is placed into the battery of the die, and the screw is tightly pressed and screwed for sealing. After sealing, the Li-In/Li In all solid state can be obtained3InCl6+Li10GeP2S12/LiNiCoMn+Li3InCl6+ C secondary battery.
The performance of the batteries of examples and comparative examples was tested and the results are shown in tables 1 to 6.
TABLE 1 comparison of conductivity of interfacial wetting agents with lithium salt as a LiTFSI solvent
TABLE 2 comparison of electrochemical windows for different interface wetting agents
TABLE 3 comparison of thermal decomposition temperatures of different interface wetting agents
TABLE 4 comparison of conductivities of different lithium salt interfacial wetting agents
TABLE 5 comparison of conductivity of LiTFSI interfacial wetting agents at different concentrations
Table 6 ionic conductivity of the interfacial wetting agent mixed with a halide solid electrolyte in example 7
Analysis table 1 shows that when the C chain is greater than 4, the conductivity of the interfacial wetting agent is very low and the interfacial wetting agent cannot be used in a solid-state battery, and therefore an ether solvent having a C chain of 4 or less is selected.
Analysis table 2 shows that, compared with LiTFSI, when LiFSI is used as the lithium salt in the interfacial wetting agent, the oxidation potential is reduced and is lower than 4.0V (when LiFSI is a single lithium salt), which is not suitable for high-voltage anode material systems such as halide solid electrolytes with a wide voltage range, high nickel, rich lithium manganese base and the like; analysis Table 4 shows that LiPF6LiBOB and liddob are insoluble in ether solvents; LiTFSI was therefore chosen as the lithium salt.
Analysis table 3 shows that when the C chain is less than or equal to 3 (such as diethyl ether and isopropyl ether), the interfacial wetting agent has low thermal decomposition stability and poor safety, and the use of the interfacial wetting agent in the battery coating process is limited; it was concluded, in conjunction with table 2, that the interfacial wetting agent performs best when the C chain is 4 (i.e., n-butyl ether or iso-butyl ether).
An analysis table 5 shows that when the concentration of the LiTFSI is between 2 and 3mol/L, the conductivity of the interfacial wetting agent is higher; as the concentration of the LiTFSI increases, the conductivity of the interfacial wetting agent tends to increase first and then decrease; therefore, the concentration range of LiTFSI is selected to be 2-3 mol/L.
Analysis table 6 shows that the conductivity retention rate of the interface wetting agent after soaking in the halide solid electrolyte is 78.3%; analysis of fig. 1 reveals that the halide solid electrolyte has no structural change after being soaked in the interfacial wetting agent for 1 d; therefore, the interface wetting agent and the halide solid electrolyte can exist stably.
FIG. 2 shows that the specific first discharge capacity of the battery with the halide solid electrolyte-high nickel cathode material system is increased from 166.9mAh/g to 209.4mAh/g after the interfacial wetting agent is added.
Fig. 3 shows that the melting capacity retention after 50 weeks of cycle is improved from 26.2% to 83.4% after the interface wetting agent is added to the battery with the halide solid electrolyte-high nickel positive electrode material system.
Fig. 4 shows that the interface resistance is significantly reduced by adding the interface wetting agent to the halide solid electrolyte-high nickel positive electrode material system battery.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. An interface wetting agent for a halide solid electrolyte is characterized in that raw materials for preparing the interface wetting agent comprise a solvent and a lithium salt, wherein the solvent is one or two of n-butyl ether or isobutyl ether; the lithium salt includes lithium bistrifluoromethanesulfonylimide.
2. The interfacial wetting agent according to claim 1, wherein the concentration of said lithium salt in said solvent is 2 to 3 mol/L.
3. The interfacial wetting agent according to claim 1 or 2, wherein said lithium salt further comprises lithium bis-fluorosulfonylimide.
4. The interfacial wetting agent according to claim 3, wherein said lithium salt is a mixture of lithium bis (trifluoromethanesulfonyl) imide and lithium bis (fluorosulfonyl) imide, and the molar percentage of lithium bis (trifluoromethanesulfonyl) imide is 50% or more.
5. The interfacial wetting agent according to any one of claims 1 to 4, wherein the chemical composition formula of the halide solid electrolyte is LiaMbXcWherein M includes at least one selected from metal elements other than Li and semimetal elements, and X includes F, Cl, Br and I.
6. The method for preparing the interfacial wetting agent according to any one of claims 1 to 5, comprising the steps of:
in a glove box filled with argon, the lithium salt was weighed, added to the solution, and completely dissolved.
7. A lithium ion battery or lithium battery containing an interfacial wetting agent, wherein the lithium ion battery or lithium battery comprises the interfacial wetting agent according to any one of claims 1 to 5.
8. The lithium ion battery or lithium battery of claim 7, wherein the lithium ion battery or lithium battery is a halide solid state electrolyte-high nickel positive electrode material system or a lithium rich manganese based high voltage positive electrode material system.
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