CN108288690B - Lithium solid-state battery cathode and preparation method and application thereof - Google Patents
Lithium solid-state battery cathode and preparation method and application thereof Download PDFInfo
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- CN108288690B CN108288690B CN201710012273.1A CN201710012273A CN108288690B CN 108288690 B CN108288690 B CN 108288690B CN 201710012273 A CN201710012273 A CN 201710012273A CN 108288690 B CN108288690 B CN 108288690B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a negative electrode of a lithium solid-state battery, a preparation method and application thereof, wherein the negative electrode comprises a negative electrode current collector and a negative electrode material loaded on the negative electrode current collector, wherein the negative electrode material comprises: a composite negative electrode active material containing metal lithium, a conductive additive, and a binder. The negative electrode provided by the invention is used in the lithium solid-state battery, so that the energy density and the safety performance of the lithium ion battery can be improved, and the problems of material pulverization, interface contact and the like are effectively relieved due to the negative electrode, so that the prepared lithium solid-state battery has better cycle performance than the lithium solid-state battery using pure metal lithium as the negative electrode.
Description
Technical Field
The invention relates to the technical field of electrochemistry and new energy materials, in particular to a negative electrode of a lithium solid-state battery, a preparation method of the negative electrode and the lithium solid-state battery comprising the negative electrode.
Background
Currently, lithium ion batteries are the highest energy density batteries among commercial batteries, and are widely used in various small electronic products, electric vehicles, and the like. In recent years, however, the rapidly developing electric automobile and energy storage industries have put higher demands on the energy density and cycle life of lithium ion batteries. In addition, lithium ion batteries have been in need of improvement in safety performance due to the use of liquid electrolytes.
In order to solve the problems of the lithium ion battery in the current market, many universities, scientific research institutes and enterprises begin to advance the development of the lithium solid-state battery. The lithium solid-state battery is mainly characterized in that metal lithium is used as a negative electrode, the energy density of the battery is greatly improved, and meanwhile, the safety performance of the battery is ensured by adopting a solid electrolyte. However, the lithium solid-state battery using pure metal lithium as the negative electrode still has the problems of material pulverization, interface contact and the like, so that the cycling performance of the battery is poor, and the practical application is difficult.
Disclosure of Invention
The invention aims to provide a novel negative electrode of a lithium solid-state battery, which is used in the lithium solid-state battery instead of pure metal lithium, and effectively relieves the problems of material pulverization, interface contact and the like in the battery, thereby improving the cycle performance of the battery. Meanwhile, compared with the lithium ion battery on the market, the lithium solid-state battery can improve the energy density and the safety performance of the battery.
The invention provides a negative electrode of a lithium solid-state battery, which comprises a negative electrode current collector and a negative electrode material loaded on the negative electrode current collector, wherein the negative electrode material comprises: a composite negative electrode active material containing metal lithium, a conductive additive, and a binder.
According to the negative electrode provided by the invention, the composite negative electrode active material containing the metal lithium comprises a mixture or a composite of the metal lithium and one or more of natural graphite, artificial graphite, mesophase micro carbon spheres (MCMB), soft carbon, hard carbon, carbon fiber, porous carbon, carbon black, graphene, carbon nanotube, lithium titanate, nano silicon, silicon-carbon composite, silicon monoxide, silicon-carbon composite, elemental tin, tin oxide and tin-cobalt-carbon. Wherein the mixture means that metallic lithium is placed between particles or on the surface of particles of other negative electrode active materials by physical mechanical mixing. The composite means that metallic lithium is placed inside particles of other negative active materials by a physical or chemical process.
According to the negative electrode provided by the invention, the conductive additive comprises one or more of acetylene black, carbon nanotubes, conductive graphite and carbon fibers.
According to the negative electrode provided by the invention, the binder comprises one or more of polyvinylidene fluoride, polytetrafluoroethylene, vinyl acetate, carboxymethyl cellulose derivatives, alginic acid, sodium alginate, polyacrylic acid, sodium polyacrylate, polyamic acid, sodium polyamide acid, polyvinyl alcohol, starch, hydroxypropyl cellulose, sodium hydroxypropyl cellulose, phenol resin, epoxy resin, polyimide, polyamide imide and styrene butadiene rubber.
According to the negative electrode provided by the invention, the current collector can be a copper foil, a copper mesh, a titanium foil, a titanium mesh, a stainless steel foil, a stainless steel mesh or a nickel mesh.
The negative electrode provided by the invention is characterized in that the composite negative electrode active material containing the metal lithium accounts for 80-99 parts by mass, the conductive additive accounts for 0-19 parts by mass, and the binder accounts for 1-20 parts by mass relative to 100 parts by mass of the negative electrode material. Preferably, the composite negative electrode active material containing lithium metal is 85 to 95 parts by mass, the conductive additive is 1 to 5 parts by mass, and the binder is 1 to 10 parts by mass, based on 100 parts by mass of the negative electrode material.
The invention also provides three preparation methods of the cathode.
In a first embodiment, the method of making comprises: under the protection of inert gas, sequentially adding a binder, a conductive additive and a composite negative electrode active substance containing metal lithium into an oil system solvent, uniformly mixing, coating on the surface of a current collector, drying, rolling and vacuumizing to prepare the negative electrode.
The inert gas comprises nitrogen and/or argon.
The oil-based solvent includes one or more of N-methylpyrrolidone, toluene, xylene, acetone, hexane, and heptane.
The drying step is to dry the pole piece coated with the slurry in an oven at the temperature of 40-200 ℃ for more than 20 minutes. Preferably, the drying temperature is 70-100 ℃, and the drying time is 1-2 hours.
The rolling step is to roll the dried pole piece by a rolling machine, wherein the pressure is 1-200000N, and preferably, the rolling pressure is 100000-150000N.
And the step of vacuumizing refers to placing the rolled pole piece in a vacuum oven, wherein the air pressure in the oven is less than or equal to 0.001Mpa, the temperature is 100-200 ℃, and the vacuumizing time is more than 2 hours. Preferably, the air pressure in the vacuumizing step is less than or equal to 0.00001Mpa, the temperature is 100-120 ℃, and the time is 12-24 hours.
In a second embodiment, the method of making comprises: adding a binder, a conductive additive and a negative active material except the metal lithium into a solvent, uniformly mixing, coating on the surface of a current collector, drying, rolling, and placing a metal lithium sheet on the surface of the pole piece to prepare the negative pole of the invention.
In a third embodiment, the method of making comprises: adding a binder, a conductive additive and a negative electrode active substance except metal lithium into a solvent, uniformly mixing, coating on the surface of a current collector, drying and rolling, then preparing the pole piece into a full battery, using an excessive lithium-containing active substance as a positive electrode of the full battery, and supplementing lithium for the negative electrode through battery charging to prepare the negative electrode of the lithium ion battery.
The invention also provides a lithium solid-state battery which comprises a positive electrode, a negative electrode and an electrolyte positioned between the positive electrode and the negative electrode, wherein the negative electrode is the negative electrode provided by the invention or the negative electrode prepared by the method.
The positive electrode includes a positive electrode active material. The positive active material comprises lithium manganate, lithium cobaltate, lithium iron phosphate and LiaCobNicMndO2(0.5<a<1.5，0<b<1，0<c<1，0<d<1)、Lia’Nib’Coc’Ald’O2(0.5<a’<1.5，0<b’<1，0<c’<1，0<d’<1)、Li2MnO3、LiNi0.5Mn1.5O4A mixture or composite of one or more of sulfur, a sulfur-carbon composite, lithium sulfide, an oxide or sulfide of cobalt, an oxide or sulfide of manganese, an oxide or sulfide of nickel, an oxide or sulfide of vanadium, and an oxide or sulfide of molybdenum.
The electrolyte comprises polyethylene oxide, polypropylene oxide, polyphosphazene and polysiliconSiloxane, polyacrylonitrile, polyvinylidene fluoride, polymethyl methacrylate, Li3xLa2/3-xTiO3(0.04＜X＜0.14)、Li3-n(OHn)Cl(0.83≤n≤2)、Li3-n(OHn)Br(1≤n≤2)、Na1+xZr2P3-xSixO12(0≤X≤3)、Li2+2xZn1-xGeO4(0＜X＜1)、Li5La3Ta2O12、Li5La3Nb2O12、Li3N、Li2S-P2S5And Li2S-SiS2A mixture or complex of one or more of (a).
The negative electrode provided by the invention is used in the lithium solid-state battery, so that the energy density and the safety performance of the lithium ion battery can be improved, and the problems of material pulverization, interface contact and the like are effectively relieved due to the negative electrode, so that the prepared lithium solid-state battery has better cycle performance than the lithium solid-state battery using pure metal lithium as the negative electrode.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a graph showing the capacity retention rate of lithium solid state batteries according to example 1 and comparative example 1 of the present invention as a function of cycle number.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
Through physical and mechanical mixing, the metal lithium powder and the silicon-carbon negative electrode material are uniformly mixed according to the mass ratio of 1:1 to prepare the composite negative electrode material containing the metal lithium. Then, in argon atmosphere, 0.5g of polyvinylidene fluoride is placed in 10g of N-methyl pyrrolidone, stirring is carried out for about 1h by using a magnetic stirrer, when the polyvinylidene fluoride is completely dissolved, 0.2g of conductive additive acetylene black is added, stirring is continued for 1h, then 9.3g of composite negative electrode material containing metal lithium is added, stirring is carried out for 4h, and the obtained slurry is coated on copper foil, wherein the thickness of the copper foil is 200 microns. And then placing the lithium ion battery in a blast oven at 80 ℃ for drying, rolling the lithium ion battery with pressure of 100000N, punching the sheet and weighing the sheet, finally performing vacuum preservation in a vacuum oven at 120 ℃ for 24 hours, transferring the sheet into a glove box, assembling the lithium ion battery by taking lithium cobaltate as a positive electrode and polyethylene oxide as electrolyte, and standing for 12 hours.
The mass energy density of the lithium solid-state battery is 320Wh/kg, and the capacity retention rate of the lithium solid-state battery is 81% after the lithium solid-state battery is cycled for 100 weeks. The change curve of the capacity retention rate along with the cycle is shown in figure 1.
Example 2
Firstly, 0.5g of polyvinylidene fluoride is placed in 10g of N-methyl pyrrolidone, stirring is carried out for about 1h by a magnetic stirrer, when the polyvinylidene fluoride is completely dissolved, 0.2g of conductive additive acetylene black is added, stirring is continued for 1h, then 9.3g of silicon-carbon negative electrode material is added, stirring is carried out for 4h, and the obtained slurry is coated on a copper foil with the thickness of 200 mu m. Then placing the mixture in a blast oven at 80 ℃ for drying, rolling the mixture by using pressure of 100000N, punching the mixture into sheets and weighing the sheets, finally preserving the sheets in a vacuum oven at 120 ℃ for 24 hours in vacuum, and transferring the sheets to a glove box for assembly. In the assembling process, a thin lithium sheet is placed on the surface of the prepared silicon-carbon negative pole piece, the whole body is used as a negative pole, lithium cobaltate is used as a positive pole, polyethylene oxide is used as electrolyte, and the lithium solid-state battery is assembled and kept stand for 12 hours.
The detection shows that the mass energy density of the lithium solid-state battery is 315Wh/kg, and the capacity retention rate of the lithium solid-state battery is 80% after 100 cycles.
Example 3
Firstly, 0.5g of polyvinylidene fluoride is placed in 10g of N-methyl pyrrolidone, stirring is carried out for about 1h by a magnetic stirrer, when the polyvinylidene fluoride is completely dissolved, 0.2g of conductive additive acetylene black is added, stirring is continued for 1h, then 9.3g of silicon-carbon negative electrode material is added, stirring is carried out for 4h, and the obtained slurry is coated on a copper foil with the thickness of 200 mu m. And then placing the lithium ion battery in a blast oven at 80 ℃ for drying, rolling the lithium ion battery with pressure of 100000N, punching the sheet and weighing the sheet, finally performing vacuum preservation in a vacuum oven at 120 ℃ for 24 hours, transferring the sheet into a glove box, assembling the lithium ion battery by taking excessive lithium cobaltate as a positive electrode and polyethylene oxide as electrolyte, and standing for 12 hours.
The detection shows that the mass energy density of the lithium solid-state battery is 308Wh/kg, and the capacity retention rate of the lithium solid-state battery is 78% after 100 cycles.
Example 4
Firstly, 0.5g of polyvinylidene fluoride is placed in 10g of N-methyl pyrrolidone, stirring is carried out for about 1h by a magnetic stirrer, when the polyvinylidene fluoride is completely dissolved, 0.2g of conductive additive acetylene black is added, stirring is continued for 1h, then 9.3g of silicon-carbon negative electrode material is added, stirring is carried out for 4h, and the obtained slurry is coated on a copper foil with the thickness of 200 mu m. Then placing the mixture in a blast oven at 80 ℃ for drying, rolling the mixture by using pressure of 100000N, punching and weighing the mixture, finally preserving the mixture in a vacuum oven at 120 ℃ for 24 hours in vacuum, transferring the mixture into a glove box, and then adding Li into lithium cobaltate2MnO3Or Li2FeO2As a positive electrode additive, the lithium content of the positive electrode was excessive, and a lithium solid state battery was assembled with this whole as the positive electrode and polyethylene oxide as the electrolyte, and left to stand for 12 hours.
The detection shows that the mass energy density of the lithium solid-state battery is 310Wh/kg, and the capacity retention rate of the lithium solid-state battery is 79 percent after the lithium solid-state battery is cycled for 100 weeks.
Comparative example 1
In the glove box, a lithium solid-state battery is assembled by taking a metal lithium sheet as a negative electrode, lithium cobaltate as a positive electrode and polyethylene oxide as an electrolyte, and is kept stand for 12 hours. The detection shows that the mass energy density of the lithium solid-state battery is 350Wh/kg, and the capacity retention rate of the lithium solid-state battery is 21% after 100 cycles.
The change curve of the capacity retention rate along with the cycle is shown in figure 1.
As can be seen from the comparison of the curves of example 1 and comparative example 1 in fig. 1, the negative electrode of the lithium solid-state battery provided by the present invention can significantly improve the cycle performance of the lithium solid-state battery.
Claims (8)
1. A negative electrode for a lithium solid-state battery, characterized in that the negative electrode comprises a negative electrode current collector and a negative electrode material supported on the negative electrode current collector, wherein the negative electrode material comprises: a composite negative electrode active material containing metal lithium, a conductive additive, and a binder; the lithium metal is prepared by: adding a binder, a conductive additive and a negative electrode active substance except metal lithium into a solvent, uniformly mixing, coating on the surface of a current collector, drying and rolling to form a negative electrode, and adding an excessive lithium-containing active substance into the positive electrode to form a positive electrode, wherein the positive electrode and the negative electrode are used for supplementing lithium to form the overall battery constructed together in the battery charging process; the composite negative electrode active material containing metal lithium is 80-99 parts by mass, the conductive additive is 0-19 parts by mass, and the binder is 1-20 parts by mass, relative to 100 parts by mass of the negative electrode material.
2. The anode according to claim 1, wherein the composite anode active material containing metallic lithium comprises a mixture or composite of metallic lithium and one or more of natural graphite, artificial graphite, mesophase carbon microbeads, soft carbon, hard carbon, carbon fibers, porous carbon, carbon black, graphene, carbon nanotubes, lithium titanate, nano-silicon, silicon-carbon composite, silicon monoxide, silicon-carbon composite, elemental tin, tin oxide, and tin-cobalt-carbon.
3. The anode of claim 1, wherein the conductive additive comprises one or more of acetylene black, carbon nanotubes, conductive graphite, and carbon fibers.
4. The negative electrode of claim 1, wherein the binder comprises one or more of polyvinylidene fluoride, polytetrafluoroethylene, vinyl acetate, carboxymethylcellulose derivatives, alginic acid, sodium alginate, polyacrylic acid, sodium polyacrylate, polyamic acid, sodium polyamide, polyvinyl alcohol, starch, hydroxypropyl cellulose, sodium hydroxypropyl cellulose, phenol resin, epoxy resin, polyimide, polyamideimide, and styrene butadiene rubber.
5. The negative electrode of claim 1, wherein the current collector is a copper foil, a copper mesh, a titanium foil, a titanium mesh, a stainless steel foil, a stainless steel mesh, or a nickel mesh.
6. The negative electrode according to claim 1, wherein the composite negative electrode active material containing lithium metal is 85 to 95 parts by mass, the conductive additive is 1 to 5 parts by mass, and the binder is 1 to 10 parts by mass, based on 100 parts by mass of the negative electrode material.
7. A method for producing the negative electrode according to any one of claims 1 to 6, characterized by comprising: adding a binder, a conductive additive and a negative electrode active substance except for metal lithium into a solvent, uniformly mixing, coating on the surface of a current collector, drying and rolling, making a pole piece into a full battery, taking an excessive lithium-containing active substance as a positive electrode of the full battery, and supplementing lithium for the negative electrode through battery charging to prepare the negative electrode.
8. A lithium solid-state battery comprising a positive electrode, a negative electrode and an electrolyte between the positive electrode and the negative electrode, wherein the negative electrode is the negative electrode according to any one of claims 1 to 6 or the negative electrode obtained by the method according to claim 7.
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| CN109037679A (en) * | 2018-08-01 | 2018-12-18 | 桑德集团有限公司 | Petroleum coke base porous carbon materials and preparation method thereof and silicon-carbon cathode material |
| CN109738823B (en) * | 2018-12-29 | 2021-03-05 | 中国科学院物理研究所 | Method for testing and evaluating performance of electrolyte system of silicon-based negative electrode half cell |
| CN111509204B (en) * | 2020-04-20 | 2021-08-06 | 中国科学院宁波材料技术与工程研究所 | Preparation method of metal lithium composite negative electrode |
| CN112038579A (en) * | 2020-09-28 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Metal lithium composite electrode, preparation method thereof and electrochemical energy storage device |
| CN113851656B (en) * | 2021-09-26 | 2023-08-15 | 珠海冠宇电池股份有限公司 | Negative electrode piece and lithium ion battery comprising same |
| CN113948674A (en) * | 2021-10-28 | 2022-01-18 | 郑州中科新兴产业技术研究院 | Safe lithium supplement negative plate, preparation method and lithium battery |
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