CN111816836A - Composite lithium metal negative electrode material and preparation method thereof - Google Patents
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Abstract
The invention discloses a composite lithium metal negative electrode material and a preparation method thereof, wherein the preparation method comprises the following steps: under the inert atmosphere, adding metal lithium and other metals into an alloy smelting furnace for smelting; keeping the temperature unchanged, and adding an electric field with certain strength into a smelting furnace to uniformly distribute elements in the molten liquid to obtain first molten liquid; adding an Mxene material to the first molten liquid; keeping the temperature and the voltage unchanged, and continuously keeping for 1-5 hours to obtain a second molten liquid; pouring the second molten liquid into a mold, cooling to room temperature, placing the mold in a magnetic field, and cooling to obtain the composite metal lithium plate; and molding the metal lithium plate to obtain the composite metal lithium belt with controllable thickness. The prepared composite negative electrode material obviously improves the rate capability and the cycle life, and obviously improves the problem of lithium dendrite, so that the safety performance of the battery is greatly improved.
Description
Technical scheme
The invention relates to the technical field of lithium batteries, in particular to a composite lithium metal negative electrode material and a preparation method thereof.
Background
With the continuous development of science and technology, the demand for high energy density power sources is higher and higher, and batteries that can theoretically provide high energy density at present include lithium air batteries, lithium sulfur batteries and lithium metal batteries, which are considered as the most promising next-generation high specific energy batteries. The metallic lithium negative electrode is considered as the most potential negative electrode material with extremely high theoretical specific capacity (3860mAh g < -1 >) and extremely negative potential (-3.040Vvs standard hydrogen electrode).
However, the large-scale application of metallic lithium negative electrodes still has many problems: in the charging and discharging process, because of the high activity of the metal lithium negative electrode and the uneven deposition of lithium ions, lithium dendrite is very easily grown on the surface, so that the diaphragm is pierced to cause short circuit to cause thermal runaway, serious safety accidents are brought, meanwhile, "dead lithium" formed after the dendrite is broken can reduce the coulomb efficiency, the characteristic that the metal lithium has no framework in the charging and discharging process can generate huge volume change to cause the instability of the negative electrode structure, the material pulverization is caused, and the service life of the battery is shortened. These problems greatly limit the practical application of lithium negative electrodes.
In recent years, researchers have solved a number of problems faced by lithium metal anodes from a number of aspects, including: the method comprises the steps of optimizing the components of the electrolyte, forming a metal lithium surface protective film, artificially building SEI (solid electrolyte interphase), constructing a three-dimensional structure negative electrode and the like, wherein the optimization of the components of the electrolyte can obviously increase the cost of the battery, the consumption of an electrolyte additive can only delay the generation of lithium dendrites, the difficulty of the surface protective layer is that the large-scale industrialized uniform interface layer preparation and the introduction of a new interface can cause the increase of the impedance of the battery and the reduction of the energy density, the preparation method and the process required by the three-dimensional nano structure negative electrode are relatively difficult, and the. Therefore, a material that can suppress the formation of lithium dendrites and that is easily prepared for a three-dimensional lithium metal negative electrode is a key to the practical use of lithium metal batteries. The lithium alloy can form a three-dimensional framework to form a good ionic and electronic conductive network, so that the lithium alloy is beneficial to uniform deposition of metal lithium, formation of lithium dendrites is inhibited, volume expansion in the charging and discharging process is reduced, and the battery cycle life is promoted, so that the lithium alloy is widely concerned.
With the demand for high energy density power supplies becoming higher and higher, numerous researchers have focused on lithium metal negative electrode materials, and although the mass energy density is improved to a certain extent, the problems still remain unsolved: because of the high activity of the metal lithium cathode and the uneven deposition of lithium ions, lithium dendrites are very easy to grow on the surface, so that the diaphragm is pierced to cause short circuit and cause thermal runaway, serious safety accidents are caused, meanwhile, dead lithium formed after the dendrites are fractured can reduce the coulomb efficiency, the self frameless characteristic of the metal lithium in the charging and discharging process can generate huge volume change to cause the instability of a cathode structure, the material pulverization is caused, and the service life of the battery is shortened. In the previous research work, a great deal of research is carried out on the series of problems, but the series of problems are still not well solved from the root.
Disclosure of Invention
In order to solve the technical problems, the invention provides a composite lithium metal negative electrode material and a preparation method thereof, the prepared composite negative electrode material obviously improves the rate capability and the cycle life, and obviously improves the problem of lithium dendrite, so that the safety performance of a battery is greatly improved.
In order to achieve the technical effects, the invention provides the following technical scheme:
a preparation method of a composite lithium metal negative electrode material comprises the following steps:
(1) under the inert atmosphere, adding metal lithium and other metals into an alloy smelting furnace for smelting;
(2) keeping the temperature unchanged, and adding an electric field with certain strength into a smelting furnace to uniformly distribute elements in the molten liquid to obtain first molten liquid;
(3) adding an Mxene material to the first molten liquid; the amount of the additive is controlled to be 5-20 wt% of the total mass of the negative electrode material; keeping the temperature and the voltage unchanged, and continuously keeping for 1-5 hours to obtain a second molten liquid;
(4) pouring the second molten liquid into a mold, cooling to room temperature, placing the mold in a magnetic field, and cooling to obtain the composite metal lithium plate;
(5) and molding the metal lithium plate to obtain the composite metal lithium belt with controllable thickness.
The further technical scheme is that other metals in the step (1) are selected from one or more of Mg, Zn and Sn, the smelting temperatures of lithium and different metals are different, wherein Li and Mg are smelted at 200-650 ℃, Li and Zn are smelted at 400-800 ℃, and Li and Sn are smelted at 300-800 ℃.
The further technical scheme is that the adding amount of other metals in the step (1) is 1-50 wt% of the total mass of the negative electrode material.
The further technical scheme is that the voltage of the external electric field in the step (2) is 0.5-3V, and the time is 0.5-2 h.
The further technical scheme is that the magnetic field intensity in the step (4) is 0.1-0.5T.
The further technical scheme is that the molding mode in the step (5) is any one of cutting, hot pressing and rolling.
The further technical scheme is that the thickness of the composite metal lithium plate in the step (5) is 20-400 microns.
The further technical scheme is that the steps (1) to (5) are carried out in a drying chamber with a dew point of less than-40 ℃ or a glove box filled with argon/helium.
The invention also provides a composite lithium metal negative electrode material prepared by the preparation method.
Mxene is a two-dimensional crystal of transition metal carbides, with a structure similar to graphene. Has a chemical formula of Mn+ 1XnWhere n is 1, 2 or 3, M is an early transition metal element such as Sc, Ti, V, Nb, etc., and X is carbon or/and nitrogen. The material has good conductivity, low ion diffusion resistance, low open circuit voltage and high lithium storage capacity, and is very suitable for being used as a negative electrode material of a metal lithium battery.
The method comprises the following steps that metal lithium and other metals are melted to form an alloy, segregation phenomena are difficult to control in melting and cooling processes, so that elements in the alloy are unevenly distributed, the material has lower mechanical strength and uneven distribution of metal lithium nucleation sites, and finally lithium dendrites are generated;
preparation of higher Li+The diffusion coefficient alloy material can promote the diffusion of lithium ions in the electrode by utilizing the metal lithium alloy phase, so that the metal lithium can perform nucleation and growth in the electrode, the deposition uniformity of the metal lithium is increased, the generation of lithium dendrites is avoided, and the safety of the battery is improved;
the Mxene material with a high lithium ion diffusion coefficient is added, so that the rapid movement of lithium ions in the composite negative electrode is facilitated, abundant lithium-philic functional groups on the surface of the Mxene contribute to the nucleation of metal lithium, and the removal and deposition of the metal lithium are promoted, so that the multiplying power performance of the material is improved, the large-rate discharge of a battery is facilitated, the formation of dendrites is inhibited, the local current density of the negative electrode is reduced by utilizing the three-dimensional framework structure of the alloy and the Mxene, the volume expansion is inhibited, and the cycle performance of the material is improved;
compared with the prior art, the invention has the following beneficial effects: the invention utilizes the action of an electric field to ensure that the molten mixed metal lithium liquid is uniformly distributed, thereby achieving the purpose of grain refinement and obtaining a uniform mixture; the element segregation generated in the cooling process of the composite lithium metal negative electrode is inhibited by the action of a magnetic field, so that the elements in the composite material are uniformly distributed; the Mxene with good conductivity and low ion diffusion resistance is added, the lithium ion diffusion capability of the negative electrode material is enhanced, the multiplying power performance of the material is improved, meanwhile, the surface of the Mxene has rich lithium-philic functional groups, the uniform nucleation of lithium is realized, the uniform deposition of lithium ions in a lithium alloy is promoted, the generation of lithium dendrites is inhibited, the coulombic efficiency of the battery is improved, meanwhile, the large specific surface area of the Mxene material reduces the volume change of the whole material in the charging and discharging process, and the cycle life of the battery is prolonged. In conclusion, the safety and the cycle life of the composite metal lithium cathode material obtained by the method are greatly improved, and the later research and application of the metal lithium cathode are facilitated.
Drawings
FIG. 1 is a schematic diagram of the preparation process of the composite lithium metal negative electrode material of the present invention.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1
Adding metal lithium and magnesium into an alloy smelting furnace in an argon environment, wherein the amount of Mg is 15 wt.%, adding an electric field of 0.5V into the heating furnace at the smelting temperature of 300 ℃, and keeping for 1 h; adding 5 wt.% of Ti3C2Tx(T ═ O, F and other functional groups); after the Mxene material is added, continuing to maintain the voltage for 1.5h until the whole molten mixed solution is uniformly mixed; pouring the mixture into a mold, cooling to room temperature, putting the whole mold in a magnetic field with the magnetic field intensity of 0.1T, cooling to room temperature, and taking out to obtain the composite metal lithium plate; rolling the composite metal lithium plate to obtain a composite metal lithium belt with the thickness of 60 microns; and (4) slicing by using a slicing machine to obtain the composite metal lithium cathode suitable for assembling the battery. In an inert atmosphere glove box, NCM811 is used as an electrode positive plate, and 1M LiPF is adopted6The electrolyte of the solution (EC) of (1) to (1) is assembled into a 2032 button cell, and then electrochemical performance test is carried out; assembly of Li-Li pair cells, DME using 1M LiTFSI: a solution of DOL 1:1 (by volume) as electrolyte containing 2 wt.% lithium nitrate as additive was assembled into 2032 coin cells for electrochemical testing.
Example 2
Adding metal lithium and zinc into an alloy smelting furnace in an argon environment, wherein the amount of Zn is 20 wt.%, and adding a 1V electric field into a heating furnace at the smelting temperature of 400 ℃ for 0.5 h; 10 wt.% of Ti was added3C2Tx(T ═ O, F and other functional groups); after the Mxene material is added, continuing to maintain the voltage for 2h until the whole molten mixed solution is uniformly mixed; pouring the mixture into a mold, cooling to room temperature, putting the whole mold in a magnetic field with the magnetic field intensity of 0.3T, cooling to room temperature, and taking out to obtain the composite metal lithium plate; rolling the composite metal lithium plate to obtain a composite metal lithium belt with the thickness of 100 microns; and (4) slicing by using a slicing machine to obtain the composite metal lithium cathode suitable for assembling the battery. In an inert atmosphere glove box, NCM811 is used as an electrode positive plate, and 1M LiPF is adopted6The electrolyte of the solution (EC) of (1) to (1) is assembled into a 2032 button cell, and then electrochemical performance test is carried out; assembly of Li-Li pair cells, DME using 1M LiTFSI: a solution of DOL 1:1 (by volume) as electrolyte containing 2 wt.% lithium nitrate as additive was assembled into 2032 coin cells for electrochemical testing.
Example 3
Adding metal lithium and tin into an alloy smelting furnace in an argon environment, wherein the amount of Sn is 30 wt.%, adding an electric field of 1.5V into the heating furnace at the smelting temperature of 550 ℃, and keeping for 1 h; adding 8 wt.% of Ti3C2Tx(T ═ O, F and other functional groups); after the Mxene material is added, continuing to maintain the voltage for 2h until the whole molten mixed solution is uniformly mixed; pouring the mixture into a mold, cooling to room temperature, putting the whole mold in a magnetic field with the magnetic field intensity of 0.5T, cooling to room temperature, and taking out to obtain the composite metal lithium plate; rolling the composite metal lithium plate to obtain a composite metal lithium belt with the thickness of 120 microns; and (4) slicing by using a slicing machine to obtain the composite metal lithium cathode suitable for assembling the battery. In an inert atmosphere glove box, NCM811 is used as an electrode positive plate, and 1M LiPF is adopted6The electrolyte of the solution (EC) of (1) to (1) is assembled into a 2032 button cell, and then electrochemical performance test is carried out; assembly of Li-Li pair cells, DME using 1M LiTFSI: a solution of DOL 1:1 (by volume) as electrolyte containing 2 wt.% lithium nitrate as additive was assembled into 2032 coin cells for electrochemical testing.
Example 4
Adding metal lithium, zinc and magnesium into an alloy smelting furnace in an argon environment, wherein the amount of Mg is 10 wt.%, the amount of Zn is 20 wt.%, and adding an electric field of 1.5V into the heating furnace at the smelting temperature of 450 ℃ for 2 hours; 10 wt.% of Ti was added3C2Tx(T ═ O, F and other functional groups); after the Mxene material is added, continuing to maintain the voltage for 3h until the whole molten mixed solution is uniformly mixed; pouring the mixture into a mold, cooling to room temperature, putting the whole mold in a magnetic field with the magnetic field intensity of 0.3T, cooling to room temperature, and taking out to obtain the composite metal lithium plate; rolling the composite metal lithium plate to obtain a composite metal lithium belt with the thickness of 100 microns; and (4) slicing by using a slicing machine to obtain the composite metal lithium cathode suitable for assembling the battery. In an inert atmosphere glove box, NCM811 is used as an electrode positive plate, and 1M LiPF is adopted6The electrolyte of the solution (EC) of (1) to (1) is assembled into a 2032 button cell, and then electrochemical performance test is carried out; assembly of Li-Li pair cells, DME using 1 MLiTFSI: a solution of DOL 1:1 (by volume) as electrolyte containing 2 wt.% lithium nitrate as additive was assembled into 2032 coin cells for electrochemical testing.
Example 5
Adding lithium, tin and magnesium into an alloy smelting furnace in an argon environment, wherein the amount of Mg is 5 wt.%, the amount of Sn is 30 wt.%, and adding an electric field of 1.5V into the heating furnace at the smelting temperature of 600 ℃ for 2 hours; 10 wt.% of Ti was added3C2Tx(T ═ O, F and other functional groups); after the Mxene material is added, continuing to maintain the voltage for 2.5h until the whole molten mixed solution is uniformly mixed; pouring the mixture into a mold, cooling to room temperature, putting the whole mold in a magnetic field with the magnetic field intensity of 0.2T, cooling to room temperature, and taking out to obtain the composite metal lithium plate; rolling the composite metal lithium plate to obtain a composite metal lithium belt with the thickness of 150 microns; and (4) slicing by using a slicing machine to obtain the composite metal lithium cathode suitable for assembling the battery. In an inert atmosphere glove box, NCM811 is used as an electrode positive plate, and 1M LiPF is adopted6Is prepared from the solution of EC, DMC and DMC in 1:1:1 as electrolyte2032 button cell, followed by electrochemical performance testing; assembly of Li-Li pair cells, DME using 1 MLiTFSI: a solution of DOL 1:1 (by volume) as electrolyte containing 2 wt.% lithium nitrate as additive was assembled into 2032 coin cells for electrochemical testing.
Example 6
Adding lithium, zinc and tin into an alloy smelting furnace in an argon environment, wherein the amount of Sn is 25 wt.%, the amount of Zn is 15 wt.%, and an electric field of 1V is added into the heating furnace at the smelting temperature of 600 ℃ and is kept for 2 hours; 10 wt.% of Ti was added3C2Tx(T ═ O, F and other functional groups); after the Mxene material is added, continuing to maintain the voltage for 3h until the whole molten mixed solution is uniformly mixed; pouring the mixture into a mold, cooling to room temperature, putting the whole mold in a magnetic field with the magnetic field intensity of 0.3T, cooling to room temperature, and taking out to obtain the composite metal lithium plate; rolling the composite metal lithium plate to obtain a composite metal lithium belt with the thickness of 120 microns; and (4) slicing by using a slicing machine to obtain the composite metal lithium cathode suitable for assembling the battery. In an inert atmosphere glove box, NCM811 is used as an electrode positive plate, and 1M LiPF is adopted6The electrolyte of the solution (EC) of (1) to (1) is assembled into a 2032 button cell, and then electrochemical performance test is carried out; assembly of Li-Li pair cells, DME using 1M LiTFSI: a solution of DOL 1:1 (by volume) as electrolyte containing 2 wt.% lithium nitrate as additive was assembled into 2032 coin cells for electrochemical testing.
The electrochemical tests of examples 1-6 and the comparative example are shown in tables 1-3, wherein Table 1 is the time voltage test result of Li-Li counter electrode in the examples and the comparative example, and the loading capacity of the positive electrode material is 15mg cm-2The multiplying power is 0.2C; table 2 shows the results of the rate capability test of examples and comparative examples; NCM811 is used as a positive electrode, 10 circles of tests are carried out under each multiplying power, and the average value of the discharge capacity of the test is taken as a calculation reference; table 3 shows the results of the electrochemical cycle performance tests in the examples and the comparative examples, under the following test conditions: current density 1mA cm-2Capacity of 5mAh cm-2。
TABLE 1 Li-Li counter electrode time-voltage test results in examples and comparative examples
TABLE 2 results of rate performance test of examples and comparative examples
Table 3 results of electrochemical cycle performance test in examples and comparative examples
As can be seen from the data in tables 1 to 3, the safety and the cycle life of the composite lithium metal anode material obtained by the method are greatly improved, which is beneficial to the later research and application of the lithium metal anode.
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (9)
1. The preparation method of the composite lithium metal negative electrode material is characterized by comprising the following steps of:
(1) under the inert atmosphere, adding metal lithium and other metals into an alloy smelting furnace for smelting;
(2) keeping the temperature unchanged, and adding an electric field with certain strength into a smelting furnace to uniformly distribute elements in the molten liquid to obtain first molten liquid;
(3) adding an Mxene material to the first molten liquid; the amount of the additive is controlled to be 5-20 wt% of the total mass of the negative electrode material; keeping the temperature and the voltage unchanged, and continuously keeping for 1-5 hours to obtain a second molten liquid;
(4) pouring the second molten liquid into a mold, cooling to room temperature, placing the mold in a magnetic field, and cooling to obtain the composite metal lithium plate;
(5) and molding the metal lithium plate to obtain the composite metal lithium belt with controllable thickness.
2. The preparation method of the composite lithium metal cathode material of claim 1, wherein the other metal in the step (1) is selected from one or more of Mg, Zn and Sn, the melting temperature of lithium is different from that of different metals, wherein Li and Mg are melted at 200-650 ℃, Li and Zn are melted at 400-800 ℃, and Li and Sn are melted at 300-800 ℃.
3. The method for preparing the composite lithium metal anode material according to claim 1, wherein the amount of the other metal added in the step (1) is 1-50 wt% of the total mass of the anode material.
4. The method for preparing the composite lithium metal anode material according to claim 1, wherein the voltage of the applied electric field in the step (2) is 0.5-3V, and the time is 0.5-2 h.
5. The preparation method of the composite lithium metal anode material according to claim 1, wherein the magnetic field strength in the step (4) is 0.1-0.5T.
6. The method for preparing the composite lithium metal anode material according to claim 1, wherein the shaping manner in the step (5) is any one of cutting, hot pressing and rolling.
7. The preparation method of the composite lithium metal anode material according to claim 1, wherein the thickness of the composite lithium metal plate in the step (5) is 20-400 μm.
8. The method for preparing the composite lithium metal anode material according to claim 1, wherein the steps (1) to (5) are performed in a dry room with a dew point of less than-40 ℃ or in a glove box filled with argon/helium.
9. A composite lithium metal negative electrode material is characterized by being prepared by the preparation method of the composite lithium metal negative electrode material according to claims 1-8.
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| CN112958734A (en) * | 2021-02-03 | 2021-06-15 | 大连交通大学 | Preparation method and application of two-dimensional metal lithium |
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