CN117594755A - Solid lithium metal negative electrode and preparation method thereof - Google Patents
Solid lithium metal negative electrode and preparation method thereof Download PDFInfo
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- CN117594755A CN117594755A CN202311579750.4A CN202311579750A CN117594755A CN 117594755 A CN117594755 A CN 117594755A CN 202311579750 A CN202311579750 A CN 202311579750A CN 117594755 A CN117594755 A CN 117594755A
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 130
- 239000007787 solid Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000151 deposition Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000008021 deposition Effects 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000005096 rolling process Methods 0.000 claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 239000011889 copper foil Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 230000000977 initiatory effect Effects 0.000 abstract description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 238000004804 winding Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000002309 gasification Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002161 passivation Methods 0.000 description 5
- 239000011149 active material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000001502 supplementing effect Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
-
- 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
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
-
- 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
-
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0421—Methods of deposition of the material involving vapour deposition
- H01M4/0423—Physical vapour deposition
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium ion batteries, and discloses a solid lithium metal negative electrode and a preparation method thereof. The method comprises the following steps: and in a vacuum environment, depositing lithium metal on the current collector through lithium metal steam, and cooling and rolling the current collector deposited with the lithium metal to obtain the solid lithium metal anode. The method can reduce the usage amount of lithium metal, the prepared solid lithium metal cathode has strong binding force, controllable thickness precision and small deposition thickness, and can increase the initial effect and the cycle life of the battery when being used in the battery.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a solid lithium metal negative electrode and a preparation method thereof.
Background
With the wide application of products such as mobile phones and notebooks and the technical maturity of new energy vehicles, the demand for lithium batteries is continuously increased, and the lithium battery cathode mainly comprises a current collector (copper foil with the thickness of 5-12 microns), an active material (a material for storing lithium ions in the charging process, mainly graphite or a part of silicon materials is doped in the graphite), a binder, a dispersing agent, a conductive agent and other materials. Along with the improvement of the product endurance requirement, the energy density (the battery charge and discharge capacity which can be achieved under the unit volume/weight) of the lithium battery is also continuously improved, and the requirement on the cycle life (one cycle of one charge and discharge) is also continuously improved.
Currently, there are many directions for improving energy density and cycle life in industry, one of which is to improve first efficiency (ratio of first discharged electric quantity to first charged electric quantity) and cycle life by supplementing lithium source, and the method is collectively called lithium supplementing technology. At present, two main ways of lithium supplement for the negative electrode are: firstly, preparing carbon-coated lithium powder, uniformly spraying the powder on the surface of an active material coating of a negative electrode, and then rolling; the other is to make lithium metal into thin slices, and roll-press and compound the thin slices on the surface of the active material coating of the anode in a physical mode. However, the above-described method still has drawbacks such as carbon-coated lithium powder: the uniformity of the particle size of the granulated powder carbon-coated lithium metal and the uniformity of the carbon coating are high, and the preparation is difficult; powdered carbon-coated lithium metal easily diffuses in the air, easily causes a safety problem, and is a risk for practical production and personnel. Lithium is supplemented by a thin lithium sheet: the adhesive force after rolling is insufficient, and the pole piece is easy to fall off in the subsequent processing process of the pole piece; the initial effect and the cycle performance are improved, the amount of lithium metal is small, the thickness of the lithium metal sheet is enough within 5 microns, and the thickness is difficult to control in the process of continuously processing the lithium sheet into a coil stock; the lithium metal is soft in texture, special treatment is needed in the rolling process and the subsequent coiling material receiving process, and adhesion between the lithium sheet and the roller press as well as after coiling material receiving is avoided.
In recent years, solid-state lithium metal anode technology is also one of the important methods for improving energy density. The technology is to change the original multiple components of the negative electrode into only two parts of current collector (copper foil) and lithium metal, wherein the lithium metal replaces the original active material and other components. The preparation method of the negative electrode mainly comprises the following steps: the lithium metal is rolled into a lithium sheet/strip with the thickness of 20-100 microns, and then the current collector is subjected to bundling and physical compounding, and then the lithium sheet/strip is used as a negative electrode.
However, the preparation of the above-described anode has the following drawbacks:
(1) The prepared solid lithium metal anode has the general thickness of 20-100 microns, the thickness used by manufacturers is generally 40-60 microns, and the lithium demand is still quite large based on the thickness calculated by the thickness, and is larger than the actual theoretical demand (lithium metal is used as a supporting body and few parts participate in the reaction), so that the actual cost of unit capacity is quite high and is far larger than the current conventional graphite system. And the lithium resource is limited, so that the subsequent technical popularization is limited;
(2) The solid lithium metal anode is physically rolled and compounded together, and the ductility of the two materials is inconsistent, and the lithium metal layer has a certain thickness, so that the possibility of separation of the current collector and the lithium metal layer easily occurs at the corner position in the subsequent processing process, particularly in a winding structural mode, and the structural design and the application of the product are limited to a certain extent;
(3) The lithium metal layer in the solid lithium metal negative electrode is formed by rolling a metal roller under the pressing force, the thickness is difficult to be less than 20 microns, the difficulty is multiplied along with the reduction of the thickness, the thickness consistency is also rapidly deteriorated, and the subsequent battery performance adopting the solid lithium metal negative electrode is influenced.
Therefore, how to provide a solid lithium metal anode with strong binding force, controllable thickness precision, small deposition thickness and capability of improving the initial efficiency and the cycle life of a battery and a preparation method thereof are problems to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a solid lithium metal anode and a preparation method thereof, which can improve the safety of anode lithium supplementing production, reduce the requirement on lithium consumption, and solve the technical problems of small binding force and difficult processing caused by large deposition thickness of the solid lithium metal anode prepared by the prior art.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the solid lithium metal anode comprises the following steps:
and in a vacuum environment, depositing lithium metal on the current collector through lithium metal steam, and cooling and rolling the current collector deposited with the lithium metal to obtain the solid lithium metal anode.
Further, the vacuum degree of the vacuum environment is-70 to-110 kPa.
Further, the temperature of the lithium metal vapor is 200-1000 ℃.
Further, the saturation degree of the lithium metal vapor is 40-95%.
Further, the current collector is copper foil, the moisture of the current collector is less than or equal to 100ppm, and the speed of the current collector passing through lithium metal steam is 0.5-30 m/min.
Further, the deposition thickness of the lithium metal is 0.5 to 20 μm.
The invention also provides the solid lithium metal anode prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) The technical scheme of the invention can improve the safety of the lithium supplementing production of the cathode and reduce the requirement on the lithium consumption;
(2) The solid lithium metal negative electrode prepared by the method has strong binding force, and the structural design of the lithium battery is not limited by a lamination mode, so that the manufacturing efficiency of the lithium metal negative electrode is improved, the equipment investment of production is reduced, and the process flow is simplified;
(3) The invention can improve the consistency of the deposition thickness of lithium metal and improve the interface stability of the cathode, thereby improving the cycle performance of the battery and other properties.
Detailed Description
The invention provides a preparation method of a solid lithium metal anode, which comprises the following steps:
and in a vacuum environment, depositing lithium metal on the current collector through lithium metal steam, and cooling and rolling the current collector deposited with the lithium metal to obtain the solid lithium metal anode.
In the present invention, the vacuum degree of the vacuum environment is-70 to-110 kPa, preferably-80 to-100 kPa, and more preferably-90 kPa.
In the present invention, the temperature of the lithium metal vapor is 200 to 1000 ℃, preferably 300 to 800 ℃, and more preferably 500 to 700 ℃.
In the present invention, the saturation degree of the lithium metal vapor is 40 to 95%, preferably 50 to 80%, and more preferably 60 to 70%.
In the invention, the current collector is copper foil, and the moisture of the current collector is less than or equal to 100ppm, preferably less than or equal to 80ppm, and more preferably less than or equal to 60ppm; the speed of the current collector passing through the lithium metal vapor is 0.5-30 m/min, preferably 3-15 m/min, and more preferably 5-10 m/min.
In the present invention, the deposition thickness of the lithium metal is 0.5 to 20. Mu.m, preferably 2 to 15. Mu.m, more preferably 5 to 10. Mu.m.
The invention also provides the solid lithium metal anode prepared by the preparation method.
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
And (3) after the lithium metal is purified and pretreated, the lithium metal is placed in a vacuum environment, the vacuum degree in the environment is gradually reduced to-70 kPa, then the lithium metal is heated to 300 ℃ to enable the lithium metal to reach a gasification state, the saturation of lithium metal steam in the environment is controlled to be 45%, a baked copper foil (the moisture is controlled to be less than 100 ppm) passes through the steam state lithium metal, the speed is controlled to be 5m/min, the deposition thickness of the lithium metal is 2 mu m, and then the solid lithium metal anode is obtained after cooling passivation and winding.
Example 2
And (3) after the lithium metal is purified and pretreated, the lithium metal is placed in a vacuum environment, the vacuum degree in the environment is gradually reduced to-80 kPa, then the lithium metal is heated to 500 ℃ to enable the lithium metal to reach a gasification state, the saturation of lithium metal steam in the environment is controlled to be 60%, a baked copper foil (the moisture is controlled to be below 90 ppm) passes through the steam state lithium metal, the speed is controlled to be 3m/min, the deposition thickness of the lithium metal is 5 mu m, and then the solid lithium metal anode is obtained after cooling passivation and winding.
Example 3
And (3) after the lithium metal is purified and pretreated, the lithium metal is placed in a vacuum environment, the vacuum degree in the environment is gradually reduced to-90 kPa, then the lithium metal is heated to 600 ℃ to enable the lithium metal to reach a gasification state, the saturation of lithium metal steam in the environment is controlled to be 75%, a baked copper foil (the moisture is controlled to be below 80 ppm) passes through the steam-state lithium metal, the speed is controlled to be 6m/min, the deposition thickness of the lithium metal is 10 mu m, and then the solid lithium metal anode is obtained after cooling passivation and winding.
Example 4
And (3) after the lithium metal is purified and pretreated, the lithium metal is placed in a vacuum environment, the vacuum degree in the environment is gradually reduced to-100 kPa, then the lithium metal is heated to 800 ℃ to enable the lithium metal to reach a gasification state, the saturation of lithium metal steam in the environment is controlled to be 80%, a baked copper foil (the moisture is controlled to be less than 100 ppm) passes through the steam lithium metal, the speed is controlled to be 10m/min, the deposition thickness of the lithium metal is 15 mu m, and then the solid lithium metal anode is obtained after cooling passivation and winding.
Example 5
And (3) after the lithium metal is purified and pretreated, the lithium metal is placed in a vacuum environment, the vacuum degree in the environment is gradually reduced to minus 110kPa, then the lithium metal is heated to 1000 ℃ to enable the lithium metal to reach a gasification state, the saturation of lithium metal steam in the environment is controlled to be 90%, a baked copper foil (the moisture is controlled to be below 70 ppm) passes through the steam lithium metal, the speed is controlled to be 15m/min, the deposition thickness of the lithium metal is 20 mu m, and then the solid lithium metal anode is obtained after cooling passivation and winding.
Performance testing
The solid lithium metal anodes obtained in examples 1 to 5 were respectively prepared into 100 lithium metal batteries, and the following performance tests were performed, and the test results are shown in table 1.
Table 1 results of performance tests of examples 1 to 5
As can be obtained from table 1, the invention can improve the consistency of the deposition thickness of lithium metal and can improve the interface stability of the anode; the capacity retention rate after 300 times of circulation at 60 ℃ is above 95%, which shows that the solid lithium metal negative electrode prepared by the method is used for preparing lithium metal batteries, and the solid batteries have good circulation performance.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. The preparation method of the solid lithium metal anode is characterized by comprising the following steps of:
and in a vacuum environment, depositing lithium metal on the current collector through lithium metal steam, and cooling and rolling the current collector deposited with the lithium metal to obtain the solid lithium metal anode.
2. The method according to claim 1, wherein the vacuum degree of the vacuum environment is-70 to-110 kPa.
3. The preparation method according to claim 1 or 2, wherein the temperature of the lithium metal vapor is 200 to 1000 ℃.
4. The method of claim 1, wherein the saturation level of the lithium metal vapor is 40-95%.
5. The method according to claim 4, wherein the current collector is copper foil, the moisture of the current collector is less than or equal to 100ppm, and the speed of passing lithium metal vapor through the current collector is 0.5-30 m/min.
6. The method according to claim 4 or 5, wherein the deposition thickness of lithium metal is 0.5 to 20 μm.
7. A solid lithium metal anode produced by the production method of any one of claims 1 to 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311579750.4A CN117594755A (en) | 2023-11-24 | 2023-11-24 | Solid lithium metal negative electrode and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311579750.4A CN117594755A (en) | 2023-11-24 | 2023-11-24 | Solid lithium metal negative electrode and preparation method thereof |
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| Publication Number | Publication Date |
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| CN117594755A true CN117594755A (en) | 2024-02-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311579750.4A Pending CN117594755A (en) | 2023-11-24 | 2023-11-24 | Solid lithium metal negative electrode and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105489845A (en) * | 2015-12-30 | 2016-04-13 | 哈尔滨工业大学 | Method for preparing thin-layer lithium metal anode for all-solid-state lithium-ion battery based on PVD |
| CN109182758A (en) * | 2018-10-22 | 2019-01-11 | 天齐锂业（江苏）有限公司 | A kind of method and system of low-grade lithium source preparation ultrathin metal lithium strip |
| CN109390548A (en) * | 2017-08-03 | 2019-02-26 | 天津中能锂业有限公司 | Secondary battery negative pole, preparation method and secondary cell |
| CN109402589A (en) * | 2019-01-02 | 2019-03-01 | 重庆天齐锂业有限责任公司 | A kind of magnetron sputtering prepares the method and system of super thin metal lithium film |
| CN114068871A (en) * | 2020-07-31 | 2022-02-18 | 天津中能锂业有限公司 | Composite belt with ultrathin lithium layers coated on two surfaces and preparation method thereof |
| KR102376634B1 (en) * | 2021-03-25 | 2022-03-22 | (주)마루엘앤씨 | Lithium deposition apparatus and deposition method for negative electrode of secondary battery |
-
2023
- 2023-11-24 CN CN202311579750.4A patent/CN117594755A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105489845A (en) * | 2015-12-30 | 2016-04-13 | 哈尔滨工业大学 | Method for preparing thin-layer lithium metal anode for all-solid-state lithium-ion battery based on PVD |
| CN109390548A (en) * | 2017-08-03 | 2019-02-26 | 天津中能锂业有限公司 | Secondary battery negative pole, preparation method and secondary cell |
| CN109182758A (en) * | 2018-10-22 | 2019-01-11 | 天齐锂业（江苏）有限公司 | A kind of method and system of low-grade lithium source preparation ultrathin metal lithium strip |
| CN109402589A (en) * | 2019-01-02 | 2019-03-01 | 重庆天齐锂业有限责任公司 | A kind of magnetron sputtering prepares the method and system of super thin metal lithium film |
| CN114068871A (en) * | 2020-07-31 | 2022-02-18 | 天津中能锂业有限公司 | Composite belt with ultrathin lithium layers coated on two surfaces and preparation method thereof |
| KR102376634B1 (en) * | 2021-03-25 | 2022-03-22 | (주)마루엘앤씨 | Lithium deposition apparatus and deposition method for negative electrode of secondary battery |
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