CN112625592A - Preparation method of lithium metal interface modification layer - Google Patents
Preparation method of lithium metal interface modification layer Download PDFInfo
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- CN112625592A CN112625592A CN202011155523.5A CN202011155523A CN112625592A CN 112625592 A CN112625592 A CN 112625592A CN 202011155523 A CN202011155523 A CN 202011155523A CN 112625592 A CN112625592 A CN 112625592A
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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Abstract
The invention provides a preparation method of a lithium metal interface modification layer, which comprises the following steps: mixing a compound with a structure shown in a formula (I), a catalyst and a solvent containing lithium salt, and stirring to obtain a mixed solution; and coating the mixed solution on a lithium foil, and carrying out heat treatment to obtain the lithium metal interface modification layer. The siloxane polymer with the structure of formula (I) is insoluble in electrolyte and small molecular monomer, and can weaken the reaction between solid electrolyte and lithium metal; the polymer is crosslinked and polymerized under the action of a catalyst to form a net structure, can inhibit the expansion of lithium metal, and has good mechanical properties. Meanwhile, the polymer skeleton is an Si-O group, so that the polymer is stable in chemical property and cannot react with lithium metal. The lithium salt can form LiN, LiF and other substances on the surface of the metal lithium, so that the density and the Young modulus of the modification layer are improved.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a lithium metal interface modification layer.
Background
Lithium metal is an important choice for future high specific energy lithium battery anodes because of its high specific capacity (3860mAh/g) and low electrochemical potential. However, lithium metal has high reactivity, SEI formed with an electrolyte is unstable, and volume expansion of lithium deposition and exfoliation processes destroys SEI (solid electrolyte interphase), forms dead lithium, and causes further consumption of the electrolyte. A modification layer is constructed on a lithium metal interface to form artificial SEI, so that lithium deposition can be improved macroscopically, and meanwhile, the interface modification layer can isolate electrolyte to a certain extent, so that harmful reaction of the electrolyte and lithium metal is reduced.
Chinese patent application No. CN109786675 discloses a ring-opening polymerization interface modification layer based on 1,3 dioxolane, which can effectively improve the rate performance and cycle life of a solid-state battery. However, the interface layer is of a linear polyether-like structure, is easily dissolved in electrolyte and monomer, and cannot be applied to liquid lithium batteries and solid battery systems based on monomer polymerization. Chinese patent application No. CN109037594A discloses a self-healing functional polymer interface modification layer, wherein the polymer can form a chelate with lithium ions on the surface of a lithium metal cathode and cover the lithium metal cathode, which not only can effectively reduce side reactions, but also can spontaneously repair the mechanical damage of the lithium cathode in the deposition/stripping process. However, toxic solvents such as tetrahydrofuran and acetone are used in the method, which is easy to cause pollution. Bauhinia et al (jacs.2018.140(37)) compared the effect of different polymer coatings (PVDF, PEO, PVDF-HFP, PU, PDMS) on lithium metal deposition, wherein PDMS (polydimethylsiloxane) with lower surface energy enables metal deposition to be more uniform, and the coulombic efficiency of the battery is also highest, reaching 99.13%. However, such PDMS has a linear structure and poor mechanical properties, and it is difficult to suppress the formation of lithium dendrites.
In summary, the current lithium metal polymer interface modification layer has the disadvantages of easy dissolution in organic solvents or monomers, poor mechanical properties, large reactivity with lithium metal, easy pollution, and the like.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for preparing a lithium metal interface modification layer, which can inhibit expansion of lithium metal, has stable chemical properties, and has high discharge capacity and coulombic efficiency.
The invention provides a preparation method of a lithium metal interface modification layer, which comprises the following steps:
mixing a compound with a structure shown in a formula (I), a catalyst and a solvent containing lithium salt, and stirring to obtain a mixed solution;
coating the mixed solution on a lithium foil, and carrying out heat treatment to obtain a lithium metal interface modification layer;
wherein x is 28-45, R1、R2Independently selected from alkyl of C1-C10.
Preferably, R1 in the compound with the structure of the formula (I) is CH3R2 is CH3And x is 38.
Preferably, the catalyst is a Karast catalyst or a chloroplatinic acid catalyst.
Preferably, the ratio of the amount of the catalyst substance to the silicon-hydrogen content in the compound with the structure of the formula (I) is 50-100 ppm.
Preferably, the lithium salt is LiNO3One or more of LiF, LiFSI or LiTFSI; the solvent is one or more of DMC and DME.
Preferably, the lithium salt accounts for 2 to 10 weight percent of the solvent; the stirring time is 20-40 min.
Preferably, the coating is blade coating, spray coating or spin coating; the thickness of the metal lithium foil is 30-100 μm.
Preferably, the temperature of the heat treatment is 50-120 ℃; the heat treatment time is 5-24 h.
The invention provides a lithium metal interface modification layer, which is prepared by the preparation method of any one of the technical schemes.
The invention provides a lithium ion battery, and a negative electrode comprises a lithium metal interface modification layer prepared by the preparation method in any one of the technical schemes.
Compared with the prior art, the invention provides a preparation method of a lithium metal interface modification layer, which comprises the following steps: mixing a compound with a structure shown in a formula (I), a catalyst and a solvent containing lithium salt, and stirring to obtain a mixed solution; and coating the mixed solution on a lithium foil, and carrying out heat treatment to obtain the lithium metal interface modification layer. The siloxane polymer with the structure of formula (I) is insoluble in electrolyte and small molecular monomer, and can weaken the reaction between solid electrolyte and lithium metal; the polymer is crosslinked and polymerized under the action of a catalyst to form a network structure, so that the expansion of lithium metal can be inhibited, and the polymer has good mechanical properties. Meanwhile, the polymer skeleton is an Si-O group, and the polymer is stable in chemical property and cannot react with lithium metal. The lithium salt can form LiN, LiF and other substances on the surface of the metal lithium, so that the density and the Young modulus of the modification layer are improved.
Drawings
FIG. 1 is a cycle diagram of a modified lithium anode;
FIG. 2 comparison of modified lithium negative electrode and pure lithium discharge capacity;
fig. 3 modified lithium negative electrode and pure lithium coulombic efficiency pairs.
Detailed Description
The invention provides a preparation method of a lithium metal interface modification layer, and a person skilled in the art can appropriately improve process parameters by referring to the content. It is expressly intended that all such alterations and modifications which are obvious to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The invention provides a preparation method of a lithium metal interface modification layer, which comprises the following steps:
mixing a compound with a structure shown in a formula (I), a catalyst and a solvent containing lithium salt, and stirring to obtain a mixed solution;
coating the mixed solution on a lithium foil, and carrying out heat treatment to obtain a lithium metal interface modification layer;
wherein x is 28-45, R1、R2Independently selected from alkyl of C1-C10.
The preparation method of the lithium metal interface modification layer provided by the invention comprises the steps of mixing the compound with the structure shown in the formula (I), the catalyst and a solvent containing lithium salt.
The compound with the structure of the formula (I) is specifically as follows:
wherein x is 28-45, preferably 28-42, and more preferably 28-32; r1、R2Independently selected from alkyl of C1-C10; preferably C1-C8 alkyl; more preferably a C1-C3 alkyl group; specifically, methyl, ethyl or propyl may be mentioned.
In the invention, the compound with the structure of the formula (I) is R1 CH3R2 is CH3And x is 38.
The compound of the formula (I) is not limited in source and can be commercially available.
The siloxane polymer with the structure of formula (I) is insoluble in electrolyte and small molecule monomer, and can weaken the reaction of solid electrolyte and lithium metal.
The catalyst of the invention is preferably a Karast catalyst or a chloroplatinic acid catalyst; the source of the present invention is not limited and may be commercially available.
The ratio of the amount of the catalyst substance to the content of silicon hydrogen in the compound with the structure of the formula (I) is preferably 50-100 ppm; more preferably 60 to 80 ppm.
The polymer is crosslinked and polymerized under the action of the catalyst to form a network structure, so that the expansion of lithium metal can be inhibited, and the polymer has good mechanical properties.
The lithium salt of the present invention isLiNO3One or more of LiF, LiFSI or LiTFSI; the solvent is one or more of DMC and DME. The present invention is not limited in its source, and may be commercially available.
Wherein, the lithium salt accounts for 2 to 10 weight percent of the solvent; more preferably 3 wt% to 9 wt%; most preferably 4 wt% to 8 wt%; particularly preferably 5 to 7 wt%.
The polymer skeleton is Si-O group, and the polymer is stable in chemical property and cannot react with lithium metal. The lithium salt can form LiN, LiF and other substances on the surface of the metal lithium, so that the density and the Young modulus of the modification layer are improved.
The mass ratio of the compound and the catalyst with the structure of formula (I) to the solvent containing lithium salt is preferably 20 wt% -40 wt%.
After mixing, the mixture was stirred at room temperature to obtain a mixed solution. The stirring time is preferably 20-40 min; more preferably 25-35 min; particularly preferably 30 min.
The mixed solution was coated on a lithium foil. The coating is preferably blade coating, spray coating or spin coating; more preferably a knife coating.
The thickness of the lithium metal foil is preferably 30-100 mu m; more preferably 30 to 90 μm; most preferably 30-70 μm.
Coating the lithium foil with the lithium interface modifier, and then carrying out heat treatment to obtain the lithium metal interface modifier.
The temperature of the heat treatment is preferably 50-120 ℃; more preferably 60-110 ℃; most preferably 70-100 ℃; particularly preferably 80-100 ℃; the time of the heat treatment is preferably 5-24 h; more preferably 6-22 h; most preferably 8-20 h; particularly preferably 8 to 12 hours.
The invention provides a lithium metal interface modification layer, which is prepared by the preparation method of any one of the technical schemes.
The preparation method of the invention has already been clearly described, and is not repeated herein.
The invention provides a lithium ion battery, and a negative electrode comprises a lithium metal interface modification layer prepared by the preparation method in any one of the technical schemes.
The lithium ion battery provided by the invention comprises a positive electrode, a negative electrode and an electrolyte. The lithium ion battery is preferably a ternary solid-state soft package battery.
The negative electrode preferably comprises the lithium metal interface modification layer prepared by the preparation method in any one of the technical schemes.
The positive electrode and the electrolyte of the present invention are not limited, and those skilled in the art will be familiar with them.
The invention provides a preparation method of a lithium metal interface modification layer, which comprises the following steps: mixing a compound with a structure shown in a formula (I), a catalyst and a solvent containing lithium salt, and stirring to obtain a mixed solution; and coating the mixed solution on a lithium foil, and carrying out heat treatment to obtain the lithium metal interface modification layer. The siloxane polymer with the structure of formula (I) is insoluble in electrolyte and small molecular monomer, and can weaken the reaction between solid electrolyte and lithium metal; the polymer is crosslinked and polymerized under the action of a catalyst to form a net structure, can inhibit the expansion of lithium metal, and has good mechanical properties. Meanwhile, the polymer skeleton is an Si-O group, so that the polymer is stable in chemical property and cannot react with lithium metal. The lithium salt can form LiN, LiF and other substances on the surface of the metal lithium, and the density and Young modulus of the modification layer are improved.
In order to further illustrate the present invention, the following will describe the preparation method of a lithium metal interface modification layer provided by the present invention in detail with reference to the following examples.
Example 1
1.5g of PMHS was added to 3g of LiNO containing 5 wt%3The solution is coated on a metal lithium foil with the thickness of 50 mu m by a blade coating mode, and then the polymer modified lithium metal cathode is obtained after heat treatment for 8 hours at the temperature of 80 ℃. Wherein in the compound of formula (I): r1 is CH3R2 is CH3And x is 38.
Assembling the ternary solid soft package battery, wherein the circulating current density is 1mA/cm2Deposition capacity 4mAh/cm2Cell cycle 32@ 90% and reference cell cycle 12@ 80%. FIGS. 1-3.
Example 2
1.5g of PMHS was added to 3g of DMC containing 5 wt% LiF, stirred at room temperature for 30min, the solution was applied by blade coating to a 50 μm thick lithium metal foil, and then heat treated at 80 ℃ for 10h to obtain a polymer-modified lithium metal negative electrode.
Assembling the ternary solid soft package battery, wherein the circulating current density is 1mA/cm2Deposition capacity 4mAh/cm2Cell cycle 40@ 90% and reference cell cycle 12@ 80%.
Example 3
1.5g of PMHS was added to 3g of DME containing 5 wt% LiFSI, stirred at room temperature for 30min, the solution was applied by blade coating to a 50 μm thick metallic lithium foil, and then heat treated at 120 ℃ for 2h to obtain a polymer-modified lithium metal negative electrode.
Assembling the ternary solid soft package battery, wherein the circulating current density is 1mA/cm2Deposition capacity 4mAh/cm2Cell cycle 45@ 90% and reference cell cycle 12@ 80%.
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 (10)
1. A preparation method of a lithium metal interface modification layer is characterized by comprising the following steps:
mixing a compound with a structure shown in a formula (I), a catalyst and a solvent containing lithium salt, and stirring to obtain a mixed solution;
coating the mixed solution on a lithium foil, and carrying out heat treatment to obtain a lithium metal interface modification layer;
wherein x is 28-45, R1、R2Independently selected from alkyl of C1-C10.
2. The method according to claim 1Wherein R1 of the compound with the structure of the formula (I) is CH3R2 is CH3And x is 38.
3. The method of claim 1, wherein the catalyst is a Karast catalyst or a chloroplatinic acid catalyst.
4. The preparation method according to claim 1, wherein the ratio of the amount of the catalyst substance to the content of silicon hydrogen in the compound having the structure of formula (I) is 50 to 100 ppm.
5. The method according to claim 1, wherein the lithium salt is LiNO3One or more of LiF, LiFSI or LiTFSI; the solvent is one or more of DMC and DME.
6. The method of claim 1, wherein the lithium salt is present in an amount of 2 to 10 wt% based on the solvent; the stirring time is 20-40 min.
7. The method according to claim 1, wherein the coating is blade coating, spray coating, or spin coating; the thickness of the metal lithium foil is 30-100 μm.
8. The method according to claim 1, wherein the heat treatment temperature is 50 to 120 ℃; the heat treatment time is 5-24 h.
9. A lithium metal interface modification layer prepared by the preparation method of any one of claims 1 to 8.
10. A lithium ion battery is characterized in that a negative electrode comprises a lithium metal interface modification layer prepared by the preparation method of any one of claims 1 to 8.
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