CN110660968A - Composite lithium metal negative electrode and preparation method thereof - Google Patents
Composite lithium metal negative electrode and preparation method thereof Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention belongs to the field of lithium batteries, and particularly relates to a composite lithium metal negative electrode and a preparation method thereof. The preparation method comprises the steps of heating the lithium metal to a molten state in an argon-protected glove box, enabling the three-dimensional carbon sheet to be in contact with the molten lithium, taking out the three-dimensional carbon sheet after the three-dimensional carbon sheet is completely soaked by the lithium metal, and cooling to room temperature to obtain the composite lithium metal cathode. The three-dimensional carbon current collector takes natural biomass catkin as a raw material, and obtains a three-dimensional carbon sheet after suction filtration and carbonization treatment. The carbonized catkin contains a large amount of heteroatoms (mainly N and O), a hollow tubular structure is kept, and molten metal lithium can be easily injected into the whole three-dimensional network through capillary action. In addition, the formed three-dimensional conductive carbon skeleton and rich space not only induce the uniform deposition of lithium, but also adapt to the volume change, thereby being beneficial to obtaining a stable lithium metal negative electrode.
Description
Technical Field
The invention belongs to the field of lithium batteries, and particularly relates to a composite lithium metal negative electrode and a preparation method thereof.
Background
Due to the limited energy density, the conventional lithium ion battery faces a great challenge in the application of electric vehicles and power grid energy storage. For developing a lithium ion battery with high energy density, a high specific capacity, stable electrode material is essential.
Lithium metal is considered to be an ideal negative electrode material due to its high theoretical specific capacity (3860mAh/g) and low redox potential (-3.04V).
However, the lithium metal negative electrode is liable to cause serious dendrite problems and large volume expansion during repeated charge and discharge cycles, resulting in sustained breakage and regeneration of a solid electrolyte interface layer (SEI), resulting in a decrease in coulombic efficiency, a rapid capacity fade, and even a serious safety hazard. These problems seriously hinder the practical use of lithium metal in high energy density secondary batteries.
During the past decades, researchers have made extensive efforts to solve the above problems, including electrolyte optimization, interface modification, and structural design. However, the former two methods cannot fundamentally inhibit the volume change of the lithium metal negative electrode in the circulation process, so in recent years, people adjust the deposition of the lithium metal through the structural design of a current collector, reduce the volume change and realize the stable circulation of the lithium metal negative electrode. Non-patent literature reports that three-dimensional porous copper current collectors are used as structural matrix of lithium metal, and the composite negative electrode obtains good cycle stability during the battery working process.
Compared with metal-based materials, the carbon-based matrix has unique advantages in the aspects of light weight, diversity and easiness in modification, and has great potential in the aspect of preparing a stable lithium metal negative electrode.
However, most three-dimensional lithium metal negative electrodes are prepared by electrochemical deposition in a battery, and then are separated/recovered, and are reused as negative electrodes in new batteries, and the process is too complicated to be suitable for large-scale practical application. Lithium is injected into the three-dimensional structure prior to battery assembly to form a composite negative electrode is an effective method.
The surface of three-dimensional current collectors, especially carbon materials, is typically lithium-phobic, which makes the incorporation of lithium difficult. In recent years, various lithium-philic modified materials, such as metals, metal oxides, Metal Organic Framework (MOF) derivatives, and surface functionalization modifications (e.g., heteroatom doping) to improve surface properties, to modulate the deposition behavior of lithium and enhance the affinity for lithium, have been explored. However, most modifications are still complex and cannot be expanded. Therefore, there is an urgent need to develop a lithium metal negative electrode having a simple operation process and stable performance.
Disclosure of Invention
The invention aims to provide a composite lithium metal negative electrode and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a composite lithium metal negative electrode comprises the following steps: and heating the lithium metal to a molten state in a glove box under the protection of argon, so that the three-dimensional carbon sheet is in contact with the molten lithium, taking out the carbon sheet after the carbon sheet is completely impregnated with the lithium metal, and cooling the carbon sheet to room temperature to obtain the composite lithium metal cathode.
The three-dimensional carbon sheet is made of natural catkin, and self-supporting catkin sheets can be obtained by cleaning and suction filtration due to the fact that fibrous structures are mutually interwoven. After carbonization, the hollow structure of the willow catkin and the three-dimensional structure of the willow catkin sheet are reserved.
The carbonization conditions are as follows: inert gases such as nitrogen, argon, helium and the like are selected for protection, the temperature is raised to 500-1500 ℃ at the speed of 1-10 ℃/min, and the heat preservation time is 1-5 h. And naturally cooling to room temperature to obtain the three-dimensional catkin carbon sheet.
The heating temperature of the lithium metal is 200-500 ℃. The viscosity is less favorable for the reaction when the temperature is increased.
The composite lithium metal negative electrode obtained by the preparation method comprises a three-dimensional carbon sheet and lithium metal filled in the three-dimensional carbon sheet, wherein the content of the lithium metal is 20% -90%.
The composite lithium metal negative electrode has the specific mass capacity of 3026mAh/g, shows small overpotential in a symmetrical battery test, and can be stably cycled for more than 500 times for a long time under the current density of 2mA/cm2, and the coulombic efficiency can still be maintained to 97.7% after 200 cycles.
Compared with the prior art, the invention has the beneficial effects that:
the three-dimensional carbon current collector takes natural biomass catkin as a raw material, and obtains a three-dimensional carbon sheet after suction filtration and carbonization treatment. The carbonized catkin contains a large amount of heteroatoms (mainly N and O), a hollow tubular structure is kept, and molten metal lithium can be easily injected into the whole three-dimensional network through capillary action. In addition, the formed three-dimensional conductive carbon skeleton and rich space not only induce the uniform deposition of lithium, but also adapt to the volume change, thereby being beneficial to obtaining a stable lithium metal negative electrode.
The composite negative electrode has a specific mass capacity of 3026mAh/g, shows a small overpotential in a symmetrical battery test, and can be stably cycled for more than 500 times for a long time under a current density of 2mA/cm2, and the coulombic efficiency can still be maintained at 97.7% after 200 cycles. In addition, the full battery with the composite metal cathode matched with the commercial lithium iron phosphate anode can realize rapid and stable charging and discharging. Compared with commercial lithium sheets, the lithium sheet has obvious advantages.
Drawings
FIG. 1 is a flow chart of the preparation of a composite lithium metal anode of the present invention;
FIG. 2 is an electrochemical plot of lithium extraction from a lithium composite metal anode at a current density of 1mA/cm 2;
FIG. 3 is a comparison of SEM images of a cycle capacity of 1mAh/cm2 cycles at a current density of 2mA/cm2 in a symmetrical cell test. a is a scanning photo of the composite lithium metal negative electrode after circulation, and b is a scanning photo of the lithium sheet after circulation;
FIG. 4 is a graph of cycle number versus voltage for a cycling capacity of 1mAh/cm2 at a current density of 2mA/cm2 in a symmetric cell test. The curve 1 is a cycle number-voltage curve of the composite lithium metal negative electrode symmetrical battery, and the curve 2 is a cycle number-voltage curve of the lithium sheet symmetrical battery.
Fig. 5 is a half-cell coulombic efficiency test curve. Graph a Current Density of 2mA/cm2, test capacity of 1mAh/cm 2. b graph Current density 2mA/cm2, test capacity 1mAh/cm 2. The curve 1 is a coulomb efficiency test curve of a half-cell assembled by a three-dimensional carbon sheet, and the curve 2 is a coulomb efficiency test curve of a half-cell assembled by a copper foil.
Fig. 6 is a discharge capacity (1 curve) and coulombic efficiency (3 curve) curve of a full battery assembled by a 5C (1C ═ 170mAh/g) composite lithium metal negative electrode and a lithium iron phosphate positive electrode, and a discharge capacity (2 curve) and coulombic efficiency (4 curve) curve of a full battery assembled by a lithium plate and a lithium iron phosphate positive electrode.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
Example 1. 0.5g of catkin was washed with deionized water, added to 150 ml of 0.5M nitric acid and stirred at 300rpm for 10 h. Vacuum filtering to obtain catkin slice, and drying the slice in vacuum oven at 80 deg.C for 10 hr. And (3) putting the thin sheet into a tube furnace, heating to 800 ℃ at a speed of 5 ℃/min under an argon atmosphere, preserving heat for 2h, and naturally cooling to room temperature to obtain the three-dimensional thin carbon sheet. Heating the lithium sheet to 300 ℃ for melting, putting the carbon sheet into the lithium sheet, taking out the lithium sheet after the lithium metal is completely soaked, and naturally cooling the lithium sheet to room temperature to obtain the composite lithium metal cathode, wherein the content of the lithium metal is 83%. Fig. 1 shows a flow chart for the preparation of a composite lithium metal anode;
the composite lithium metal negative electrode and a counter electrode lithium sheet are assembled into a battery, the battery is discharged to 1V under the current density of 1mA/cm2, and the measured mass specific capacity is up to 3026mAh/g as shown in figure 2. The electrolyte is 1M 1, 3-Dioxolane (DOL)/ethylene glycol dimethyl ether (DME) (volume ratio is 1:1) solution of lithium bistrifluoromethanesulfonimide (LiTFSI).
A symmetric battery was assembled using a composite lithium metal negative electrode for charge-discharge cycling at a current density of 2mA/cm2 and a capacity of 1mAh/cm 2. The cycle number-voltage curve of the composite lithium metal negative electrode is shown as curve 1 in fig. 3, and the electrolyte is 1M 1, 3-Dioxolane (DOL)/ethylene glycol dimethyl ether (DME) (volume ratio is 1:1) solution of lithium bistrifluoromethanesulfonylimide (LiTFSI). The symmetric cell was assembled using lithium plates for charge and discharge cycling with other conditions unchanged and the cycle number-voltage curve is shown as curve 2 in fig. 3.
The composite lithium metal negative electrode symmetric battery and the lithium sheet symmetric battery after 200 cycles of cycling are disassembled for scanning electron microscope test, as shown in fig. 4. The picture A is a picture of the composite lithium metal negative electrode plate after being cycled for 200 circles, and the picture b is a picture of the lithium plate after being cycled for 200 circles.
A coulombic efficiency test is carried out on a battery assembled by a three-dimensional carbon sheet, a copper foil and a lithium sheet, and an electrolyte is a 1, 3-Dioxolane (DOL)/ethylene glycol dimethyl ether (DME) (volume ratio is 1:1) solution of 1M lithium bistrifluoromethanesulfonylimide (LiTFSI). As shown in FIG. 5a, curve 1, under the conditions of current density of 2mA/cm2 and capacity of 1mAh/cm2, the coulombic efficiency of 97.7 percent can still be maintained after 200 circles of test of the three-dimensional carbon sheet. The coulomb efficiency of the battery using the copper foil as the current collector is sharply reduced after 50 circles (curve 2); when the current density is 5mA/cm2 and the capacity is 1mAh/cm2, the coulombic efficiency of the battery assembled by using the three-dimensional carbon sheets is still 97.5 percent after 100 cycles, as shown in a curve 1 of a figure 5b, and the coulombic efficiency is obviously better than that of the battery using a copper foil as a current collector under the same condition (a curve 2).
The discharge specific capacity (curve) and coulombic efficiency curve of the full battery assembled by the composite lithium metal negative electrode and the lithium iron phosphate positive electrode are shown in fig. 6. After the material is circulated for 250 circles under the high current density of 5C, the capacity retention rate of 82 percent still exists; the full battery assembled by using a pure lithium sheet as the cathode lithium iron phosphate anode has the full battery discharge specific capacity (curve) and coulombic efficiency curve assembled by the composite lithium metal cathode and the lithium iron phosphate anode as shown in fig. 6, and the discharge specific capacity begins to be greatly attenuated after 100 cycles under the same condition. The used lithium iron phosphate positive active material: the mass ratio of the conductive agent Super P to the adhesive PVDF is 7:2:1, and the surface loading of the active substance is about 4mg/cm 2.
The electrolyte used was a 1M (LiPF6) solution of Ethylene Carbonate (EC) and diethyl carbonate (DEC) (1:1 by volume).
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (6)
1. The preparation method of the composite lithium metal negative electrode is characterized by comprising the following steps of: and heating the lithium metal to a molten state in a glove box under the protection of argon, so that the three-dimensional carbon sheet is in contact with the molten lithium, taking out the three-dimensional carbon sheet after the three-dimensional carbon sheet is completely impregnated with the lithium metal, and cooling the three-dimensional carbon sheet to room temperature to obtain the composite lithium metal cathode.
2. The method for preparing the composite lithium metal anode of claim 1, wherein the three-dimensional carbon sheet is made of natural catkin, and is cleaned and filtered to obtain a self-supporting catkin sheet due to interweaving of fibrous structures; the willow catkin sheet is carbonized, and the hollow structure of the willow catkin and the three-dimensional structure of the willow catkin sheet are reserved to obtain the three-dimensional carbon sheet.
3. The method of preparing the composite lithium metal negative electrode according to claim 2, wherein the carbonization conditions of the willow flocculus are as follows: under the protection of inert gas, heating to 500-; and naturally cooling to room temperature to obtain the three-dimensional catkin carbon sheet.
4. The method of claim 1, wherein the heating temperature of the lithium metal is 200-500 ℃.
5. The composite lithium metal negative electrode obtained by the preparation method of any one of claims 1 to 4, which comprises a three-dimensional carbon sheet and lithium metal filled in the three-dimensional carbon sheet, wherein the content of the lithium metal is 20 to 90 percent.
6. The lithium metal composite anode as claimed in claim 5, wherein the lithium metal composite anode has a specific mass capacity of up to 3026mAh/g, shows a small overpotential in a symmetrical battery test, and can be stably cycled for more than 500 times for a long time under a current density of 2mA/cm2, and the coulombic efficiency can still be maintained at 97.7% after 200 cycles.
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Cited By (8)
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| CN111261833A (en) * | 2020-01-19 | 2020-06-09 | 中南大学 | Self-supporting lithium metal cathode and preparation and application thereof |
| CN112072167A (en) * | 2020-09-10 | 2020-12-11 | 五邑大学 | Method for compounding metal lithium and carbon nano tube for inorganic solid-state lithium metal battery |
| CN112750986A (en) * | 2020-12-31 | 2021-05-04 | 华东理工大学 | Metallic lithium cathode with high-ionic-conductivity artificial SEI film and preparation method thereof |
| CN112909234A (en) * | 2021-01-20 | 2021-06-04 | 合肥工业大学 | Preparation method and application of lithium cathode or sodium cathode |
| CN113903889A (en) * | 2020-07-06 | 2022-01-07 | 厦门大学 | Lithium metal negative electrode and preparation method and application thereof |
| CN114512637A (en) * | 2022-01-20 | 2022-05-17 | 武汉工程大学 | Three-dimensional composite lithium metal cathode with multifunctional interface layer and preparation method thereof |
| CN115020657A (en) * | 2022-07-27 | 2022-09-06 | 西安交通大学 | Alkali metal composite cathode and integrated preparation method thereof |
| CN115172759A (en) * | 2022-09-06 | 2022-10-11 | 深圳海润新能源科技有限公司 | Current collector, battery, current collector preparation method and battery preparation method |
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| CN115172759A (en) * | 2022-09-06 | 2022-10-11 | 深圳海润新能源科技有限公司 | Current collector, battery, current collector preparation method and battery preparation method |
| CN115172759B (en) * | 2022-09-06 | 2022-12-20 | 深圳海润新能源科技有限公司 | Current collector, battery, current collector preparation method and battery preparation method |
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