CN114744190A - Additive for preventing partial lithium supplement excess of pre-lithiation negative electrode, method thereof and lithium ion battery - Google Patents
Additive for preventing partial lithium supplement excess of pre-lithiation negative electrode, method thereof and lithium ion battery Download PDFInfo
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- CN114744190A CN114744190A CN202210283153.6A CN202210283153A CN114744190A CN 114744190 A CN114744190 A CN 114744190A CN 202210283153 A CN202210283153 A CN 202210283153A CN 114744190 A CN114744190 A CN 114744190A
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 81
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000000654 additive Substances 0.000 title claims abstract description 51
- 230000000996 additive effect Effects 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 40
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 27
- 239000013589 supplement Substances 0.000 title claims abstract description 22
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000006138 lithiation reaction Methods 0.000 title abstract description 5
- 239000003792 electrolyte Substances 0.000 claims abstract description 23
- 150000001450 anions Chemical class 0.000 claims abstract description 18
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 230000009469 supplementation Effects 0.000 claims description 8
- 125000000129 anionic group Chemical group 0.000 claims description 4
- 229910001914 chlorine tetroxide Inorganic materials 0.000 claims description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Chemical compound [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 claims description 2
- 230000001502 supplementing effect Effects 0.000 abstract description 17
- 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
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 239000011888 foil Substances 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000243 solution Substances 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
- 238000013329 compounding Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying 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
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000009751 slip forming Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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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
- H01M10/42—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
- 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 partial lithium supplement excess of a pre-lithiation negative electrode, a method thereof and a lithium ion battery. The additive of the invention is added with anion additive with oxidizability into electrolyte, and the anion additive with oxidizability can generate oxidation-reduction reaction with metallic Li to oxidize the metallic Li into Li+. Therefore, in addition to the electrochemical oxidation reaction of the metallic lithium close to the graphite in the electrolyte in the lithium supplementing process, the metallic lithium close to the side of the electrolyte can simultaneously react with the anions, and the products are all Li+. During the circulation process, lithium precipitated from the local lithium supplementing excess region cannot be converted into Li through electrochemical oxidation reaction+But can be converted to Li by chemical oxidation+。
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, relates to a lithium supplement additive, and particularly relates to an additive for preventing partial lithium supplement of a pre-lithiation negative electrode from being excessive, a method of the additive and a lithium ion battery.
Background
Since the advent of lithium ion batteries, lithium ion batteries have been rapidly developed and have been the subject of major development of rechargeable batteries. With the popularization of new energy industries such as energy storage and the like, the requirements of power type and energy storage type lithium ion batteries are remarkably increased.
The lithium ion battery mainly comprises a positive electrode, a negative electrode, a diaphragm, electrolyte, a shell, a lug and the like, wherein lithium ions are completely stored in a positive electrode active material and the electrolyte serving as an ion conductor before formation. The formation is to charge the battery cell for the first time after the battery is injected with liquid, activate active substances in the battery and activate the lithium ion battery. During the formation process, the solvent and lithium salt in the electrolyte can generate side reaction with the negative electrode to form a solid electrolyte interface film (SEI).
A plurality of charge-discharge cycles are required for a complete formation process, and research shows that 10% of the initial capacity of the lithium ion battery is used as irreversible capacity loss to form an SEI film in the first charge-discharge cycle, and a small amount of SEI film is continuously formed in the subsequent cycles. Since lithium ions from the positive electrode are consumed in the formation process and cannot become active lithium capable of providing effective capacity for the battery cell, various lithium supplement technologies are paid attention.
Chinese patent 201610015441.8 developed a method of compounding a layer of lithium metal foil on the negative electrode to supplement lithium, chinese patent 201710438908.4 disclosed a method of supplementing lithium by using lithium metal vapor to evaporate a lithium layer with a thickness less than 1 micron, and patent application 201910452204.1 also used a method of metal lithium vapor to evaporate, which continuously heats the lithium vapor pipe, avoids deposition, and improves the process. Chinese patent 201210351225.2 discloses a method of applying an organic lithium salt to the surface of a negative electrode sheet in an inert gas, so that lithium ions in the organic lithium salt are reduced to metallic lithium and inserted into the negative electrode sheet, and then drying the negative electrode sheet.
The most effective negative electrode lithium supplementing technology in the prior art is lithium supplementing by using a metal lithium foil, and because of the process and other reasons, the negative electrode covered with a microporous lithium foil on the whole surface has excessive lithium supplementing, and the lithium supplementing amount is controlled by adopting a method of a strip-shaped or net-shaped microporous lithium foil in the actual production process.
However, since the lateral conduction of lithium ions in graphite is difficult, the lithium is replenished excessively in the part covered by the lithium foil, and only a small amount in the part not covered by the lithium foil, which easily results in analyzing lithium in the part covered by the lithium foil during the subsequent cycle.
Disclosure of Invention
Aiming at the problem of excessive local lithium supplement of the stripe-shaped or net-shaped microporous lithium foil, the invention designs the additive for preventing the excessive local lithium supplement of the pre-lithiation cathode, and can promote the rapid lithium dissolution in the lithium supplement process and the dissolution of lithium separated out in the subsequent cycle process, thereby preventing the problem of local lithium separation caused by the excessive local lithium supplement.
The invention also provides a method for supplementing lithium by using the additive and a lithium ion battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
an additive for preventing partial lithium supplement excess of a prelithiated negative electrode is an oxidizing anionic additive, and the addition amount of the additive is 0.05-2 mol/L.
In the invention, oxidizing anion additives are added into the electrolyte, and the oxidizing anion additives can perform oxidation-reduction reaction with metallic Li to oxidize the metallic Li into Li+. Therefore, in addition to the electrochemical oxidation reaction of the metallic lithium close to the graphite in the electrolyte in the lithium supplementing process, the metallic lithium close to the side of the electrolyte can simultaneously react with the anions, and the products are all Li+. During the circulation process, lithium precipitated from the local lithium supplementing excess region cannot be converted into Li through electrochemical oxidation reaction+But can be converted to Li by chemical oxidation+。
As a preferable mode of the present invention, the additive is added in an amount of 0.05 to 1.5 mol/L.
As a preferable mode of the present invention, the additive is added in an amount of 0.1 to 1 mol/L.
As a preferred embodiment of the present invention, the anion of the oxidizing anion additive is selected from I3 -、ClO4 -、MnO4 -、Cr2O7 2-Or [ Fe (CN)6]3-。
In a preferred embodiment of the present invention, the anion of the anionic additive with oxidation is [ Fe (CN) ]6]3-。
In this embodiment, the anion selection principle of the present invention [ Fe (CN) ]6]3-The principle is as follows:
Li+[Fe(CN)6]3-＝Li++[Fe(CN)6]4-。
[Fe(CN)6]4-diffused to the surface of the positive lithium iron phosphate to generate [ Fe (CN) ]6]3-：
Li++[Fe(CN)6]4-+FePO4＝LiFePO4+[Fe(CN)6]3-
[Fe(CN)6]3-Continuously diffusing to the negative electrode to react with the lithium metal, and circulating.
In a second aspect, the invention provides a method for preventing local lithium overdose of a prelithiated negative electrode comprising the above additive.
In a preferred embodiment of the present invention, the method comprises adding an oxidizing anionic additive to the electrolyte, and standing the electrolyte after injection.
As a preferable scheme of the invention, the standing time is 24-360h at 45 ℃ after the liquid injection.
In a third aspect, the invention provides a lithium ion battery comprising the above additive.
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 supplement;
2) the additive can promote the rapid dissolution of lithium in the lithium supplementing process and the dissolution of lithium separated out in the subsequent circulating process;
3) the lithium supplementing method is simple and effective, low in cost, simple in requirements on operating environment and better in effect.
Drawings
Figure 1 is the full electrical anatomical interface of example 1.
Fig. 2 is the full electrical anatomical interface of comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present invention, all the components are known in the art unless otherwise specified.
Example 1
This example provides an additive and method for preventing over-lithium supplementation of a pre-lithiated negative electrode by adding 1mol/L of Li to the electrolyte3[Fe(CN)6]And standing for 24 hours at 45 ℃ after liquid injection to obtain the lithium-supplement cathode with a complete interface.
Example 2
This example provides an additive and method for preventing over-lithium supplementation of a pre-lithiated negative electrode, which includes adding 1.2mol/L of Li to the electrolyte3[Fe(CN)6]And standing for 24 hours at 45 ℃ after liquid injection to obtain the lithium-supplement cathode with a complete interface.
Example 3
This example provides an additive and method for preventing over-lithium supplementation of a pre-lithiated negative electrode, which includes adding 1mol/L of Li to the electrolyte3[Fe(CN)6]And standing for 24 hours at 25 ℃ after liquid injection to obtain the lithium-supplement cathode with a complete interface.
Example 4
This example provides for preventing prelithiation of the negative electrodeAn additive for locally supplementing excessive Li is prepared through adding Li (1 mol/L) to electrolyte3[Fe(CN)6]And standing for 360 hours at 25 ℃ after liquid injection to obtain the lithium-supplement cathode with a complete interface.
Example 5
This example provides an additive and method for preventing over-lithium supplementation of a pre-lithiated negative electrode, which includes adding 0.1mol/L of Li to the electrolyte3[Fe(CN)6]And standing for 24 hours at 45 ℃ after liquid injection to obtain the lithium-supplement cathode with a complete interface.
Example 6
This example provides an additive and method for preventing over-lithium supplementation of a pre-lithiated negative electrode, which includes adding 0.5mol/L of Li to the electrolyte3[Fe(CN)6]And standing for 24 hours at 45 ℃ after liquid injection to obtain the lithium-supplement cathode with a complete interface.
Comparative example 1, in the electrolyte, Li was not added3[Fe(CN)6]Standing at 45 deg.C for 24 hr.
Referring to fig. 1 and 2, when the cross sections of example 1 and comparative example 1 in the full-electrical state are seen, the phenomenon of lithium precipitation at the stripes on the surface of example 1 is obviously reduced, while the phenomenon of lithium precipitation at the stripes on the surface of comparative example 1 is severe, which indicates that Li is generated3[Fe(CN)6]The addition of the additive promotes the dissolution of the lithium metal.
It can be seen that the electrolyte is added with the anion additive with the oxidizing property, and the anion additive with the oxidizing property can generate oxidation-reduction reaction with metallic Li to oxidize the metallic Li into Li+. Therefore, in addition to the electrochemical oxidation reaction of the metallic lithium close to the graphite in the electrolyte in the lithium supplementing process, the metallic lithium close to the side of the electrolyte can simultaneously react with the anions, and the products are all Li+. During the circulation process, lithium precipitated from the local lithium supplementing excess region cannot be converted into Li through electrochemical oxidation reaction+But can be converted to Li by chemical oxidation+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, thereby preventing the problem of local lithium precipitation caused by excessive local lithium supplementing.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.
Claims (9)
1. An additive for preventing partial lithium supplement excess of a prelithiated negative electrode is characterized in that the additive is an oxidizing anion additive, and the addition amount of the additive is 0.05-2 mol/L.
2. The additive for preventing partial lithium supplementation of a prelithiated negative electrode as recited in claim 1, wherein the additive is added in an amount of 0.05 to 1.5 mol/L.
3. The additive for preventing partial lithium supplementation of a prelithiated negative electrode as recited in claim 1, wherein the additive is added in an amount of 0.1 to 1 mol/L.
4. Additive for preventing local lithium replenishment of a prelithiated negative electrode as claimed in claim 1, 2 or 3, wherein the anion of the oxidic anionic additive is selected from the group consisting of I3 -、ClO4 -、MnO4 -、Cr2O7 2-Or [ Fe (CN)6]3-。
5. The additive for preventing partial lithium supplementation of a prelithiated negative electrode as claimed in claim 4, wherein the additive is characterized by the fact thatIn the oxidizing anion additive, the anion is [ Fe (CN) ]6]3-。
6. A method for preventing local lithium replenishment of a prelithiated negative electrode in excess, comprising the additive of any of claims 1 to 5.
7. The method for preventing the partial lithium supplement of the prelithiation negative electrode as claimed in claim 6, wherein the method comprises adding an oxidizing anion additive to the electrolyte, and standing after the electrolyte injection.
8. The method for preventing the partial lithium supplement excess of the prelithiation negative electrode according to claim 7, wherein the standing time after the liquid injection is 24-360h at 45 ℃.
9. A lithium ion battery comprising the additive of any one of claims 1 to 5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210283153.6A CN114744190A (en) | 2022-03-22 | 2022-03-22 | Additive for preventing partial lithium supplement excess of pre-lithiation negative electrode, method thereof and lithium ion battery |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210283153.6A CN114744190A (en) | 2022-03-22 | 2022-03-22 | Additive for preventing partial lithium supplement excess of pre-lithiation negative electrode, method thereof and lithium ion battery |
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| CN105024113A (en) * | 2015-07-10 | 2015-11-04 | 苏州迪思伏新能源科技有限公司 | Preparation method of rechargeable lithium ion oxygen battery based on lithium-intercalated graphite |
| CN108878974A (en) * | 2017-05-16 | 2018-11-23 | 中信国安盟固利动力科技有限公司 | A kind of lithium ion battery mends lithium electrolyte and mends lithium method |
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| CN111900478A (en) * | 2020-08-20 | 2020-11-06 | 江苏师范大学 | Electrolyte additive, electrolyte containing electrolyte additive and lithium metal battery containing electrolyte |
| CN112072078A (en) * | 2020-09-15 | 2020-12-11 | 昆山宝创新能源科技有限公司 | Pre-lithiated negative plate and preparation method and application thereof |
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| CN113659203A (en) * | 2021-07-18 | 2021-11-16 | 哈尔滨工业大学 | Electrolyte containing composite additive and application thereof |
| CN114024024A (en) * | 2021-11-04 | 2022-02-08 | 安徽工业大学 | Electrolyte additive, application thereof and lithium metal battery |
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2022
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Patent Citations (8)
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| CN105024113A (en) * | 2015-07-10 | 2015-11-04 | 苏州迪思伏新能源科技有限公司 | Preparation method of rechargeable lithium ion oxygen battery based on lithium-intercalated graphite |
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