CN114744190B - Additive for preventing excessive lithium supplement of pre-lithiated cathode and method thereof and lithium ion battery - Google Patents
Additive for preventing excessive lithium supplement of pre-lithiated cathode and method thereof and lithium ion battery Download PDFInfo
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- CN114744190B CN114744190B CN202210283153.6A CN202210283153A CN114744190B CN 114744190 B CN114744190 B CN 114744190B CN 202210283153 A CN202210283153 A CN 202210283153A CN 114744190 B CN114744190 B CN 114744190B
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 96
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000000654 additive Substances 0.000 title claims abstract description 47
- 230000000996 additive effect Effects 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000013589 supplement Substances 0.000 title claims abstract description 12
- 239000003792 electrolyte Substances 0.000 claims abstract description 19
- 125000000129 anionic group Chemical group 0.000 claims abstract description 11
- 150000001450 anions Chemical class 0.000 claims abstract description 8
- 230000009469 supplementation Effects 0.000 claims description 16
- 239000011888 foil Substances 0.000 claims description 14
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 230000001502 supplementing effect Effects 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000006056 electrooxidation reaction Methods 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010439 graphite Substances 0.000 abstract description 4
- 229910002804 graphite Inorganic materials 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 238000006479 redox reaction Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 238000004090 dissolution Methods 0.000 description 7
- 238000007792 addition Methods 0.000 description 6
- 230000001590 oxidative effect Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001914 chlorine tetroxide Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Chemical compound [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000002904 solvent 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- 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
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses an additive for preventing excessive lithium supplement of a pre-lithiated negative electrode locally, a method thereof and a lithium ion battery. The additive of the invention adds an anionic additive with oxidability to the electrolyte, and the anionic additive with oxidability can perform oxidation-reduction reaction with metal Li to oxidize the metal lithium into Li +. Therefore, in the lithium supplementing process, except that the metallic lithium close to the graphite is subjected to electrochemical oxidation reaction in the electrolyte, the metallic lithium close to the solution side can simultaneously react with the anions, and the product is Li +. During the cycling, the lithium precipitated in the region where the excess lithium is locally supplied cannot be converted into Li + by electrochemical oxidation reaction, but can be converted into Li + by chemical oxidation.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, relates to a lithium supplementing additive, and particularly relates to an additive for preventing excessive local lithium supplementing of a pre-lithiated negative electrode, a method thereof and a lithium ion battery.
Background
Since the advent of lithium ion batteries, rapid developments have been made, which have become the key development targets for rechargeable batteries. Along with popularization of new energy industries such as energy storage, the demands of power type and energy storage type lithium ion batteries are obviously increased.
The lithium ion battery mainly comprises a positive electrode, a negative electrode, a diaphragm, electrolyte, a shell, a tab and the like, wherein all lithium ions are stored in the positive electrode active material and the electrolyte serving as an ion conductor before formation. The formation is that the battery is charged for the first time after the liquid injection is completed, and active substances in the battery are activated, so that the lithium ion battery is activated. In the formation process, the solvent and lithium salt in the electrolyte can react with the negative electrode to form a solid electrolyte interface film (SEI).
A complete formation process requires multiple charge and discharge cycles, and studies have shown that in the first charge and discharge cycle, 10% of the initial capacity of a lithium ion battery is lost as irreversible capacity to form an SEI film, and a small amount of SEI film continues to be formed in subsequent cycles. Since lithium ions from the positive electrode are consumed during the formation process, they cannot be used as active lithium that can provide an effective capacity for the battery cell, and various lithium supplementing techniques have been paid attention.
Chinese patent 201610015441.8 developed a method of lithium supplementation by compounding a layer of lithium metal foil on the negative electrode, chinese patent 201710438908.4 discloses a lithium supplementation method of vapor deposition of lithium metal to a thickness of less than 1 micron, and patent application 201910452204.1 also uses a method of vapor deposition of lithium metal to continuously heat the lithium vapor pipe, avoid deposition and improve the process. The method of Chinese patent 201210351225.2 is to apply organic lithium salt to the surface of the negative plate in inert gas, so that lithium ions in the organic lithium salt are reduced into metal lithium and are embedded into the negative plate, and then the negative plate is dried.
The most effective negative electrode lithium supplementing technology is that metal lithium foil is used for supplementing lithium, and the negative electrode of the microporous lithium foil is covered on the whole surface for excessive lithium supplementing due to the reasons of technology and the like, so that the lithium supplementing amount is controlled by adopting a stripe-shaped or net-shaped microporous lithium foil method in the actual production process.
However, since the lateral conduction of lithium ions in graphite is very difficult, the part covered with the lithium foil is excessively supplemented with lithium, while the part not covered with the lithium foil is only slightly supplemented with lithium, which easily results in the part covered with the lithium foil being partially supplemented with lithium during the subsequent cycle.
Disclosure of Invention
Aiming at the problem of excessive local lithium supplement of the striped or meshed microporous lithium foil, the invention designs the additive for preventing excessive local lithium supplement of the pre-lithiated cathode, which can promote the rapid dissolution of lithium in the lithium supplement process and the dissolution of precipitated lithium in the subsequent circulation process, thereby preventing the problem of local lithium precipitation caused by excessive local lithium supplement.
The invention also provides a lithium supplementing method and a lithium ion battery using the additive.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
An additive for preventing the pre-lithiated cathode from being excessively supplemented with lithium locally, wherein the additive is an anionic additive with oxidability, and the addition amount of the additive is 0.05-2mol/L.
In the present invention, an oxidizing anionic additive is added to the electrolyte, and these oxidizing anionic additives can undergo oxidation-reduction reaction with metallic Li to oxidize the metallic lithium into Li +. Therefore, in the lithium supplementing process, except that the metallic lithium close to the graphite is subjected to electrochemical oxidation reaction in the electrolyte, the metallic lithium close to the solution side can simultaneously react with the anions, and the product is Li +. During the cycling, the lithium precipitated in the region where the excess lithium is locally supplied cannot be converted into Li + by electrochemical oxidation reaction, but can be converted into Li + by chemical oxidation.
As a preferable mode of the invention, the addition amount of the additive is 0.05-1.5mol/L.
As a preferable mode of the invention, the addition amount of the additive is 0.1-1mol/L.
As a preferred embodiment of the present invention, the anions in the oxidic anionic additive are selected from I 3 -、ClO4 -、MnO4 -、Cr2O7 2- or [ Fe (CN) 6]3- ].
As a preferred embodiment of the present invention, the anion in the oxidizing anion additive is [ Fe (CN) 6]3- ].
In the present technical solution, the anion selection principle [ Fe (CN) 6]3- of the present invention, its principle is:
Li+[Fe(CN)6]3-＝Li++[Fe(CN)6]4-。
The diffusion of [ Fe (CN) 6]4- to the surface of the positive lithium iron phosphate occurs as follows to produce [ Fe (CN) 6]3-:
Li++[Fe(CN)6]4-+FePO4＝LiFePO4+[Fe(CN)6]3-
[ Fe (CN) 6]3- continues to diffuse to the cathode to react with the metallic lithium, and repeats.
In a second aspect, the invention provides a method for preventing local lithium overfilling of a prelithiated anode comprising the additive described above.
As a preferred embodiment of the present invention, the method comprises adding an anionic additive having oxidizing property to the electrolyte, and standing after pouring.
As a preferable scheme of the invention, the standing time is 24-360h at 45 ℃ after liquid injection.
In a third aspect the invention provides a lithium ion battery comprising the additive described above.
Compared with the prior art, the invention has the following beneficial effects:
1) The additive can effectively inhibit local lithium precipitation caused by excessive local lithium supplementation;
2) The additive can promote the rapid dissolution of lithium in the lithium supplementing process and the dissolution of precipitated lithium in the subsequent circulating process;
3) The lithium supplementing method is simple and effective, has low cost, simple requirements on the operation environment and better effect.
Drawings
FIG. 1 is a full electroanatomical interface of example 1.
Fig. 2 is a full electroanatomical interface of comparative example 1.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, 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.
In the present invention, if not specified, they are all prior art.
Example 1
The embodiment provides an additive and a method for preventing excessive local lithium supplementation of a pre-lithiated negative electrode, wherein 1mol/L of Li 3[Fe(CN)6 is added into electrolyte, and the lithium supplementation negative electrode with a complete interface can be obtained after standing for 24 hours at 45 ℃ after liquid injection.
Example 2
The embodiment provides an additive and a method for preventing excessive local lithium supplementation of a pre-lithiated negative electrode, wherein 1.2mol/L of Li 3[Fe(CN)6 is added into electrolyte, and the lithium supplementation negative electrode with a complete interface can be obtained after standing for 24 hours at 45 ℃ after liquid injection.
Example 3
The embodiment provides an additive and a method for preventing excessive local lithium supplementation of a pre-lithiated negative electrode, wherein 1mol/L of Li 3[Fe(CN)6 is added into electrolyte, and the lithium supplementation negative electrode with a complete interface can be obtained after standing for 24 hours at 25 ℃ after liquid injection.
Example 4
The embodiment provides an additive and a method for preventing excessive local lithium supplementation of a pre-lithiated negative electrode, wherein 1mol/L of Li 3[Fe(CN)6 is added into electrolyte, and the lithium supplementation negative electrode with a complete interface can be obtained after the electrolyte is filled and then is kept stand at 25 ℃ for 360 hours.
Example 5
The embodiment provides an additive and a method for preventing excessive local lithium supplementation of a pre-lithiated negative electrode, wherein 0.1mol/L Li 3[Fe(CN)6 is added into electrolyte, and the lithium supplementation negative electrode with a complete interface can be obtained after standing for 24 hours at 45 ℃ after liquid injection.
Example 6
The embodiment provides an additive and a method for preventing excessive local lithium supplementation of a pre-lithiated negative electrode, wherein 0.5mol/L Li 3[Fe(CN)6 is added into electrolyte, and the lithium supplementation negative electrode with a complete interface can be obtained after standing for 24 hours at 45 ℃ after liquid injection.
In comparative example 1, li 3[Fe(CN)6 was not added to the electrolyte, and the mixture was left to stand at 45℃for 24 hours after the injection.
Referring to fig. 1 and 2, the lithium precipitation phenomenon at the stripes on the surface of example 1 is significantly reduced, while the lithium precipitation phenomenon at the stripes on the surface of comparative example 1 is serious, indicating that the addition of the Li 3[Fe(CN)6 additive promotes the dissolution of metallic lithium, as seen in the cross-sections of full state of example 1 and comparative example 1.
It follows that the addition of anionic additives with oxidizing properties to the electrolyte can undergo a redox reaction with metallic Li, oxidizing metallic lithium to Li +. Therefore, in the lithium supplementing process, except that the metallic lithium close to the graphite is subjected to electrochemical oxidation reaction in the electrolyte, the metallic lithium close to the solution side can simultaneously react with the anions, and the product is Li +. In the circulation process, although the lithium precipitated in the excessive area of the local lithium supplement cannot be converted into Li + through electrochemical oxidation reaction, the lithium can be converted into Li + through chemical oxidation, and the additive disclosed by the invention can promote the rapid dissolution of the lithium in the lithium supplement process and the dissolution of the precipitated lithium in the subsequent circulation process, so that the problem of local lithium precipitation caused by excessive local lithium supplement is prevented.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various modifications and additions may be made without departing from the scope of the invention. Equivalent embodiments of the present invention will be apparent to those skilled in the art having the benefit of the teachings disclosed herein, when considered in the light of the foregoing disclosure, and without departing from the spirit and scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the technical solution of the present invention.
Claims (7)
1. An additive for preventing the local lithium supplement excess of a striped or meshed microporous lithium foil prelithiation negative electrode is characterized in that the additive is an anionic additive with oxidability, the addition amount of the additive is 0.05-2mol/L, the anion in the anionic additive with oxidability is [ Fe (CN) 6]3- ], and the additive is Li 3[Fe(CN)6 ].
2. An additive for preventing local lithium overfilling of a striped or meshed microporous lithium foil prelithiated anode according to claim 1, wherein the additive is added in an amount of 0.05-1.5mol/L.
3. An additive for preventing local lithium overfilling of a striped or meshed microporous lithium foil prelithiated anode according to claim 1, wherein the additive is added in an amount of 0.1-1mol/L.
4. A method for preventing local excess lithium supplementation of a striped or reticulated microporous lithium foil prelithiated anode, comprising the additive of any one of claims 1-3.
5. The method for preventing local lithium overfilling of a striped or meshed microporous lithium foil prelithiated anode according to claim 4, wherein the method comprises adding an anionic additive with oxidability into the electrolyte, and standing after liquid injection.
6. The method for preventing excessive lithium supplement of a striped or meshed microporous lithium foil prelithiated anode locally according to claim 4, wherein the standing time is 24-360h at 45 ℃ after liquid injection.
7. A lithium ion battery comprising the additive of any one of claims 1-3.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210283153.6A CN114744190B (en) | 2022-03-22 | 2022-03-22 | Additive for preventing excessive lithium supplement of pre-lithiated cathode and method thereof and lithium ion battery |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210283153.6A CN114744190B (en) | 2022-03-22 | 2022-03-22 | Additive for preventing excessive lithium supplement of pre-lithiated cathode and method thereof and lithium ion battery |
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| CN114744190A CN114744190A (en) | 2022-07-12 |
| CN114744190B true CN114744190B (en) | 2024-06-11 |
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