CN112186153A - Lithium cathode with interface nanosheet protective layer and preparation method thereof - Google Patents
Lithium cathode with interface nanosheet protective layer and preparation method thereof Download PDFInfo
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
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Abstract
The invention discloses a lithium negative electrode with an interface nanosheet protective layer, which comprises a lithium negative electrode substrate, wherein a graphite phase carbon nitride nanosheet interface layer is covered on the surface of the lithium negative electrode substrate. The preparation method comprises the following steps: adding graphite-phase carbon nitride nanosheet powder into an organic solvent for dispersing to prepare graphite-phase carbon nitride nanosheet dispersion liquid; and dropwise coating the graphite-phase carbon nitride nanosheet dispersed liquid on the surface of a lithium negative electrode substrate, and forming a graphite-phase carbon nitride nanosheet interface layer on the surface of the lithium negative electrode after the solvent is volatilized to obtain the lithium negative electrode with the interface nanosheet protective layer. According to the invention, the graphite-phase carbon nitride nanosheet interface layer is coated on the surface of the lithium negative electrode substrate, and abundant and uniformly distributed nitrogen atoms in the graphite-phase carbon nitride nanosheets can interact with lithium ions to form transient Li-N bonds, so that the lithium ion flux is adjusted, a stable deposition process is realized, the generation of lithium dendrites and dead lithium is reduced, and the polarization is reduced.
Description
Technical Field
The invention belongs to the field of lithium ion battery materials, and particularly relates to a lithium cathode with an interface nanosheet protective layer and a preparation method thereof.
Background
Since Sony corporation commercialized lithium ion batteries in 1991, lithium ion batteries have become one of the most important technologies in current energy storage technologies. Nowadays, lithium ion batteries are widely used in the fields of portable electronic devices, electric vehicles, power station energy storage, and the like. However, over decades of development, commercial lithium ion batteries employing graphite cathodes have approached their theoretical energy density limit (250 Wh kg)-1) And the rapid increase of the energy density requirement of the battery in the field of energy storage cannot be met, so that the development of a negative electrode material with higher energy density is urgently needed.
Lithium metal negative electrodes have higher theoretical capacity (3860mAh g)-1) And a lower electrode potential (-3.04V vs. she) to form a "holy cup" of negative electrode material. Mass energy of LMO | Li battery (LMO is lithium transition metal oxide) after replacing graphite negative electrode with lithium metalThe density can reach 440Wh kg-1. Therefore, the lithium negative electrode is one of the most potential negative electrodes of next generation batteries.
However, the high reactivity of the lithium metal can continuously react with the electrolyte, so that a surface SEI film is continuously generated, and the coulombic efficiency is reduced; while the non-uniform deposition of lithium causes lithium dendrite growth to pierce the separator easily causing short circuits. Therefore, improvement in stability of the lithium negative electrode is required.
In patent publication No. CN109004276A, lithium salt, ionic liquid, inorganic nanoparticles, and lithiated Nafion polymer are mixed to prepare a lithium negative electrode protective film with good stability and ionic conductivity, but this method requires many kinds of materials and is complicated in process. In patent document CN109148826A, a magnetron sputtering method is used to prepare a LiF layer on the surface of a lithium negative electrode, so that the LiF layer has good lithium ion conductivity, but the method has high requirements on equipment, complex process and difficulty in mass production. In patent document No. CN110311093A, a graphene thin film is introduced on the surface of a lithium negative electrode to reduce interface impedance and regulate lithium uniform nucleation, but graphene lacks a functional group capable of interacting with lithium ions, and thus, the effect of uniform lithium ion deposition is weak.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings mentioned in the background technology, and provide a lithium negative electrode with an interface nanosheet protective layer and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a lithium negative electrode with an interface nanosheet protective layer comprises a lithium negative electrode substrate, wherein a graphite-phase carbon nitride nanosheet interface layer covers the surface of the lithium negative electrode substrate.
The lithium negative electrode preferably has a graphite-phase carbon nitride nanosheet loading of 0.01-1mg cm on the lithium negative electrode substrate-2。
In the lithium negative electrode, the interface layer of the graphite-phase carbon nitride nanosheets preferably has a thickness of 1 to 10 μm.
As a general inventive concept, the present invention also provides a preparation method of the above lithium negative electrode with the interface nanosheet protective layer, comprising the steps of:
(1) adding graphite phase carbon nitride nanosheet into organic solvent for dispersion to prepare the graphite phase carbon nitride nanosheet with the concentration of 0.1-10mg ml-1The graphite phase carbon nitride nanosheet dispersion liquid of (a);
(2) and dropwise coating the graphite-phase carbon nitride nanosheet dispersed liquid on the surface of a lithium negative electrode substrate, and forming a graphite-phase carbon nitride nanosheet interface layer on the surface of the lithium negative electrode after the solvent is volatilized to obtain the lithium negative electrode with the interface nanosheet protective layer.
In the preparation method, preferably, the graphite phase carbon nitride nanosheet is prepared by a thermal polymerization method, and the thickness of the graphite phase carbon nitride nanosheet is 1-50 nm.
In the preparation method, preferably, the specific preparation process of the graphite-phase carbon nitride nanosheet is as follows:
(a) placing urea in a ceramic crucible, covering the ceramic crucible with a cover, placing the ceramic crucible in a high-temperature furnace, heating to 400-600 ℃, and preserving heat for 1-6 hours to obtain graphite-phase carbon nitride;
(b) adding the graphite-phase carbon nitride into deionized water, dispersing the graphite-phase carbon nitride by using a cell crusher to enable the graphite-phase carbon nitride to be completely stripped into nanosheets, concentrating and drying the nanosheets to obtain graphite-phase carbon nitride nanosheet powder.
In the above preparation method, it is preferable that the time for the dispersion treatment using the cell disruptor in the step (b) is 0.5 to 24 hours.
The preparation method described above, preferably, in step (b), the concentration means that the dispersion is subjected to 1000-10000r min-1Performing centrifugal treatment for 0.1-15min at the centrifugal rotating speed.
In the above-mentioned production method, preferably, in the step (b), the drying is freeze-drying for 2 to 4 days.
In the above preparation method, preferably, in the step (1), the organic solvent is one or more selected from 1, 3-dioxolane, N-methylpyrrolidone, N, N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, tetrahydrofuran, acetonitrile and succinonitrile.
In the preparation method, preferably, in the step (1), the dispersing refers to ultrasonic dispersing, and the time of ultrasonic dispersing is 1-10 min.
Compared with the prior art, the invention has the advantages that:
(1) according to the invention, the graphite-phase carbon nitride nanosheet interface layer is coated on the surface of the lithium negative electrode substrate, and abundant and uniformly distributed nitrogen atoms in the graphite-phase carbon nitride nanosheets can interact with lithium ions to form transient Li-N bonds, so that the lithium ion flux is adjusted, a stable deposition process is realized, the generation of lithium dendrites and dead lithium is reduced, and the polarization is reduced.
(2) According to the invention, the graphite-phase carbon nitride nanosheet interface layer is coated on the surface of the lithium negative electrode substrate, the graphite-phase carbon nitride nanosheet layer is very thin, and a cavity exists in the molecular structure, so that the rapid transmission of lithium ions under high current density is facilitated.
(3) According to the invention, the graphite-phase carbon nitride nanosheet interface layer covers the surface of the lithium negative electrode substrate, and the graphite-phase carbon nitride nanosheet has low electronic conductivity and certain mechanical strength, can inhibit penetration of lithium dendrites, and can prevent short circuit of the battery.
(4) In the process of the graphite-phase carbon nitride nanosheet, the graphite-phase carbon nitride is ultrasonically stripped by the cell crusher, the cell crusher has high ultrasonic power and stripping efficiency, and the graphite-phase carbon nitride nanosheet with the thickness of only 1nm can be obtained.
(5) The invention forms the graphite phase carbon nitride interface layer on the surface of the lithium cathode by the direct dripping coating method, and the process is simple.
Drawings
FIG. 1 is a schematic representation of the reaction process for preparing graphite phase carbon nitride from urea by calcination in an embodiment of the present invention.
Fig. 2 is an atomic force microscope image of graphite phase carbon nitride nanoplates prepared in an example of the invention.
Fig. 3 is an SEM image of a cross section of a graphite phase carbon nitride modified lithium negative electrode in example 1 of the present invention.
Fig. 4 is an XPS chart of the surface of the negative electrode supporting lithium carbonitride in example 1 of the present invention.
Fig. 5 is a graph of the cycling performance of a lithium symmetrical cell of a comparative example of the present invention.
Fig. 6 is a graph of the cycling performance of a lithium symmetric battery of example 1 of the invention.
Fig. 7 is a graph of rate performance of NMC622 positive electrode full cells prepared from lithium negative electrodes of example 1 of the present invention and comparative example.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1(CN 1):
the lithium cathode with the interface nanosheet protective layer comprises a lithium sheet, wherein a layer of graphite-phase carbon nitride nanosheet is covered on the surface of the lithium sheet, and the loading capacity of the graphite-phase carbon nitride nanosheet on the lithium sheet is 0.04mg cm-2。
The preparation method of the lithium negative electrode with the interface nanosheet protective layer of the embodiment is as follows:
(1) weighing appropriate amount of urea, placing in a ceramic crucible, covering, and heating at 5 deg.C for 5min in a high temperature furnace-1Heating to 550 ℃ at the heating rate, and preserving heat for 4 hours to obtain faint yellow block graphite phase carbon nitride; grinding the obtained faint yellow block graphite phase carbon nitride into powder, and mixing a proper amount of powder with deionized water to prepare the mixture with the concentration of 1mg ml-1The solution is treated by ultrasonic wave for 1h by a cell crusher to ensure that the graphite phase carbon nitride is completely stripped into sodiumRice flakes, forming a white dispersion; centrifuging the prepared white dispersion liquid at the rotating speed of 10,000rpm for 5 minutes to obtain a concentrated solution, and finally freeze-drying the concentrated solution for 3 days to obtain white CN nano-sheet powder; the reaction process of the graphite phase carbon nitride prepared by urea through calcination is shown in figure 1, the prepared graphite phase carbon nitride has uniformly distributed nitrogen atoms, and the middle hollow space can allow lithium ions to pass through; the atomic force microscopy image is shown in FIG. 2, and the thickness of the carbon nitride nanosheet is 1.07 nm;
(2) weighing a proper amount of prepared CN nano-sheet powder, adding the CN nano-sheet powder into a 1, 3-Dioxolane (DOL) solvent to prepare the solution with the concentration of 1mg ml-1Then carrying out ultrasonic treatment for 5 minutes to obtain white dispersion liquid; then a dropper is adopted to absorb 1 drop of the prepared dispersion liquid and drop the dispersion liquid on a lithium metal cathode, after the solvent is completely volatilized, a layer of thin graphite phase carbon nitride nanosheet interface layer is attached to the surface of the lithium cathode, and the load capacity of CN is about 0.04mg cm-2。
Fig. 3 is an SEM image of the cross-section of the graphite phase carbon nitride modified lithium negative electrode in this example, and it can be seen that the thickness of the graphite phase carbon nitride interface layer is about 3 μm.
Fig. 4 is an XPS diagram of the surface of the negative electrode loaded with lithium carbonitride in this example, which shows that the interaction between lithium and nitrogen generates Li-N bonds, which can regulate the deposition/stripping process of lithium ions, and reduce battery polarization and dendrite generation.
The lithium negative electrode prepared in this example was assembled into a lithium symmetrical battery in a glove box filled with argon gas, and the lithium deposition/exfoliation performance at room temperature was tested on a battery test system. The cycling performance of the cell is shown in FIG. 6, and the symmetric cell can be at 1mA cm-2Current density of 1mAh cm-2The capacity of (a) is stable for 400h, since the lithium-philic graphitic carbon nitride stabilizes the lithium ion deposition/exfoliation process, reducing polarization and dendrite formation.
Example 2(CN 10):
the lithium negative electrode with the interface nanosheet protective layer comprises a lithium sheet, wherein a layer of graphite-phase carbon nitride nanosheet is covered on the surface of the lithium sheet, and the loading capacity of the graphite-phase carbon nitride nanosheet on the lithium sheet is0.44mg cm-2。
The preparation method of the lithium negative electrode with the interface nanosheet protective layer of the present comparative example is as follows:
(1) the preparation method for preparing the CN nanosheet powder is the same as that of example 1;
(2) weighing a proper amount of prepared CN nano-sheet powder, adding the CN nano-sheet powder into a 1, 3-Dioxolane (DOL) solvent to prepare 1mg ml of solution-1Then, carrying out ultrasonic treatment for 5 minutes by adopting an ultrasonic cleaning machine to obtain a white dispersion liquid; then a dropper is adopted to absorb 10 drops of the prepared dispersion liquid and add the dispersion liquid on a lithium metal cathode, after the solvent is completely volatilized, a layer of thin graphite phase carbon nitride nanosheet interface layer is attached to the surface of the lithium cathode after the solvent is completely volatilized, and the load capacity of CN is about 0.44mg cm-2。
The prepared lithium sheet was assembled into a lithium symmetrical battery in a glove box filled with argon gas, and the lithium deposition/exfoliation performance was tested on a battery test system at room temperature. The symmetrical battery can be at 1mA cm-2Current density of 1mAh cm-2Is cycled for 250 hours.
Comparative example 1 (Bare):
this comparative example is a blank lithium plate control.
The blank lithium sheets were assembled into lithium symmetrical cells in a glove box filled with argon and tested for lithium deposition/exfoliation performance at room temperature on a battery test system. The cycling performance of the lithium symmetrical cell is shown in FIG. 5, the cell is at 1mA cm-2Current density of 1mAh cm-2Can only circulate for about 150 hours.
The rate performance of the lithium cathodes in example 1 and comparative example 1 prepared into NMC622 positive full cells is shown in fig. 7, and example 1 has better rate performance, which shows that graphite phase carbon nitride can promote lithium ion diffusion at high current density.
Claims (9)
1. The lithium negative electrode with the interface nanosheet protective layer is characterized by comprising a lithium negative electrode substrate, wherein a graphite-phase carbon nitride nanosheet interface layer is covered on the surface of the lithium negative electrode substrate.
2. The lithium negative electrode of claim 1, wherein the loading of graphite phase carbon nitride nanoplates on the lithium negative electrode substrate is from 0.01 to 1mg cm-2。
3. The lithium negative electrode of claim 1 or 2, wherein the interface layer of graphite phase carbon nitride nanosheets has a thickness of 1-10 μ ι η.
4. A method for preparing a lithium negative electrode with an interfacial nanoplate protective layer according to any of claims 1 to 3, comprising the steps of:
(1) adding graphite phase carbon nitride nanosheet powder into an organic solvent for dispersion to prepare the graphite phase carbon nitride nanosheet powder with the concentration of 0.1-10mg ml-1The graphite phase carbon nitride nanosheet dispersion liquid of (a);
(2) and dropwise coating the graphite-phase carbon nitride nanosheet dispersed liquid on the surface of a lithium negative electrode substrate, and forming a graphite-phase carbon nitride nanosheet interface layer on the surface of the lithium negative electrode after the solvent is volatilized to obtain the lithium negative electrode with the interface nanosheet protective layer.
5. The production method according to claim 4, wherein the graphite-phase carbon nitride nanosheet powder is a graphite-phase carbon nitride nanosheet produced by a thermal polymerization process, and has a thickness of 1 to 50 nm.
6. The preparation method of claim 5, wherein the specific preparation process of the graphite-phase carbon nitride nanosheet powder is as follows:
(a) placing urea in a ceramic crucible, covering the ceramic crucible with a cover, placing the ceramic crucible in a high-temperature furnace, heating to 400-600 ℃, and preserving heat for 1-6 hours to obtain graphite-phase carbon nitride;
(b) adding the graphite-phase carbon nitride into deionized water, dispersing the graphite-phase carbon nitride by using a cell crusher to enable the graphite-phase carbon nitride to be completely stripped into nanosheets, concentrating and drying the nanosheets to obtain graphite-phase carbon nitride nanosheet powder.
7. The preparation method according to claim 6, wherein in the step (b), the dispersion treatment is carried out for 0.5 to 24 hours using a cell crusher;
concentration means that the dispersion is subjected to 1000-10000r min-1Performing centrifugal treatment for 0.1-15min at the centrifugal rotating speed;
drying refers to freeze drying, and the freeze drying time is 2-4 days.
8. The process according to any one of claims 4 to 7, wherein in step (1), the organic solvent is one or more selected from the group consisting of 1, 3-dioxolane, N-methylpyrrolidone, N, N-dimethylformamide, N, N-dimethylacetamide, dimethylsulfoxide, tetrahydrofuran, acetonitrile and succinonitrile.
9. The production method according to any one of claims 4 to 7, wherein in the step (1), the dispersion is ultrasonic dispersion, and the time for ultrasonic dispersion is 1 to 60 min.
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| CN117423919A (en) * | 2023-12-19 | 2024-01-19 | 济南中瑞泰新材料科技有限公司 | Modified lithium metal battery negative electrode and preparation method thereof |
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