CN108878974B - Lithium ion battery lithium supplement electrolyte and lithium supplement method - Google Patents
Lithium ion battery lithium supplement electrolyte and lithium supplement method Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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Abstract
The invention provides a lithium ion battery lithium supplement electrolyte and a lithium supplement method. Firstly, the lithium-supplementing electrolyte comprises an organic solvent and lithium salt, when the electrode potential is below 4.3V (vs Li +/Li), the anion of the lithium salt is unstable at the positive electrode of the lithium ion battery, an anodic oxidation decomposition reaction can occur, and an intercalation reaction of lithium ions occurs at the corresponding negative electrode. The lithium supplementing method comprises the following steps: and injecting the lithium supplement electrolyte into the lithium ion battery, pre-charging the lithium ion battery to a lithium supplement voltage to supplement lithium to the negative electrode and control the lithium supplement amount, removing the residual lithium supplement electrolyte after the lithium supplement reaction is finished, re-injecting the conventional electrolyte, and then pre-charging the battery into a working procedure. The method is simple to operate, and can accurately and uniformly supplement lithium to the negative electrode by only properly changing the battery pre-charging process without modifying the existing production line, so that the first coulomb efficiency of the battery is improved, the energy density is improved, and the cycle performance is improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a lithium ion battery lithium supplement electrolyte and a lithium supplement method.
Background
At present, materials such as graphite, hard carbon or alloy and the like capable of reversibly releasing and inserting lithium ions are generally adopted as negative electrode materials of commercial lithium ion batteries, and in the first charging process of the lithium ion batteries, a solid electrolyte interface film (SEI film) generated on the surfaces of the negative electrode materials and some side reactions consume a part of lithium ions from the positive electrode materials to form irreversible capacity, so that the first coulombic efficiency and capacity of a battery cell are reduced.
Research shows that consumed lithium ions can be supplemented by a lithium supplementing (or called pre-lithium intercalation) technology, so that the first efficiency and the energy density of the lithium ion battery are improved. For example, patent applications with publication numbers CN104993098A, CN102779975A, and CN103199217A all disclose technical solutions for introducing a lithium source into a lithium ion battery. The method mainly comprises the steps of mixing SLMP lithium metal powder with a negative electrode through a slurry mixing, rolling or coating technology, or covering a metal lithium sheet on the surface of the negative electrode sheet for lithium pre-embedding. However, the above technologies can theoretically supplement lithium to the battery cell, but when the battery cell is actually put into industrial production, many process problems are faced: the production process is complex, the operation environment is harsh, and the production line needs to be partially or even completely modified or eliminated, so that the manufacturing cost is obviously increased and the waste of the existing production equipment is wasted. Meanwhile, the lithium pre-intercalation amount and the lithium intercalation unevenness are difficult to control, so that the consistency of the battery core is poor, and the problems of lithium precipitation, serious cycle performance attenuation and the like occur. Moreover, because of the 'macroscopic' lithium intercalation mode, the lithium intercalation amount is difficult to control, the lithium intercalation range and the lithium intercalation amount have to be enlarged, the material waste and the further increase of the cost are also seriously caused, and the redundant added lithium cannot be recycled, so that the method is very unfortunately.
In view of this, it is necessary to provide a technology that is simple in operation, has low impact on existing process equipment, saves a reasonable amount of usage, and has high consistency in manufacturing products to achieve the improvement of first coulomb efficiency and capacity of the lithium ion battery.
Disclosure of Invention
The invention aims to provide a lithium ion battery lithium supplement electrolyte and a lithium supplement method, which realize controllable and uniform lithium supplement on a lithium ion battery cathode by using the lithium supplement electrolyte, simplify the production process, effectively supplement the irreversible capacity loss of the lithium ion battery, and improve the first coulombic efficiency, the cycle performance and the energy density of the lithium ion battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
a lithium ion battery lithium-supplementing electrolyte comprises an organic solution of lithium salt; when the electrode potential of the lithium ion battery anode is below 4.3V (vs Li +/Li), the anion of the lithium salt is unstable at the lithium ion battery anode, and an anodic oxidation reaction can occur to generate a by-product which is mainly gas; in this voltage range, the positive electrode material also undergoes a delithiation reaction. When the anode oxidation reaction of the lithium salt anion and the lithium removal reaction of the anode material simultaneously occur at the anode, the lithium ions of the lithium salt generate a lithium insertion reaction at the cathode. The overall result of the above reaction is to supplement lithium to the negative electrode, and is referred to as a lithium supplement reaction in the present embodiment. Meanwhile, the invention also provides a lithium ion battery lithium supplementing method, which comprises the following steps: injecting lithium-supplementing electrolyte into a lithium ion battery after packaging (after the battery is assembled and before a conventional electrolyte injection process), fully infiltrating positive and negative pole pieces and a diaphragm inside the battery with the lithium-supplementing electrolyte, charging to lithium-supplementing voltage by adopting constant current, removing the residual lithium-supplementing electrolyte after the lithium-supplementing reaction is completed, injecting conventional working electrolyte, pre-charging the battery, and other subsequent conventional processes.
Among them, the "working electrolyte" referred to in the present invention is any electrolyte that can be conventionally used in lithium ion batteries in the art. Wherein, the step of fully soaking is the same as the step of soaking by the conventional electrolyte, and the soaking is preferably 24-48 h.
Wherein the lithium salt is lithium trifluoroacetate or lithium acetate; the concentration of lithium salt is 0.1-1mol/L, and the solubility of lithium salt can be properly adjusted by adjusting the experimental temperature, wherein the temperature range is 25-60 ℃. The solvent of the organic solution is one or more of Propylene Carbonate (PC), Ethylene Carbonate (EC), Butylene Carbonate (BC), dimethyl carbonate (DMC), diethyl carbonate (DEC) and Methyl Propyl Carbonate (MPC). Also, it is preferable that the solvent is as identical as possible to the solvent contained in the conventional working electrolyte to be used later.
The injection amount of the lithium supplement electrolyte is 3g-10g/Ah, the lithium supplement current is 0.01C-0.2C, and the lithium supplement voltage is 3.75V-4.2V. The lithium supplementing amount can be controlled and adjusted through the concentration of lithium salt in the lithium supplementing electrolyte, the injection amount of the lithium supplementing electrolyte, the lithium supplementing current and the lithium supplementing voltage, so that the aim of accurately supplementing lithium is fulfilled.
The lithium supplement demand of the lithium ion battery cathode is adjusted according to the difference of the lithium ion battery anode and cathode materials, for a graphite cathode, the lithium supplement amount is 1% -30% of the battery design capacity, for a hard carbon cathode, the lithium supplement amount is 10% -40% of the battery design capacity, and for an alloy cathode with lower efficiency, the lithium supplement amount is 10% -50% of the battery design capacity.
The technical scheme provided by the invention can overcome the obstacles brought by the traditional lithium supplement technology and solve the problems of overhigh cost, harsh environmental requirements, poor safety and the like. Meanwhile, the lithium intercalation amount and the lithium intercalation uniformity can be accurately controlled, so that the irreversible capacity of the lithium ion battery is reduced, the first coulombic efficiency and the cycle life of the battery are effectively improved, the energy density of the battery is improved, and the battery has better electrochemical performance and safety. Meanwhile, the method provided by the invention is used for preparing the lithium ion battery, the operation is simple, the existing production line is not required to be modified, only the pre-charging process is required to be properly adjusted, and the cost is low. And accurate supply is accurately provided according to the lithium supply demand, so that the waste of materials and other problems possibly caused by redundant materials are avoided. Meanwhile, the recovered lithium supplement electrolyte can be recycled after corresponding treatment, and theoretically, the beneficial effect that the utilization rate of lithium salt is 100% can be achieved.
Drawings
Fig. 1 shows the charging curves of button cells a and b produced by the method of the invention (example one).
Fig. 2 is a room temperature cycle curve of a lithium ion battery prepared by the method of the present invention.
Detailed Description
The lithium ion battery lithium ion supplement electrolyte and the corresponding lithium ion supplement method of the present invention will be described in more detail with reference to the following embodiments. However, the present invention is not limited to the following examples.
The first embodiment is as follows:
at a certain temperature (30 ℃), dissolving lithium trifluoroacetate in a mixed solvent (EC: DEC ═ 1:2, volume ratio), wherein the concentration of lithium trifluoroacetate is 1mol/L, and preparing lithium trifluoroacetate lithium-supplement electrolyte. Lithium hexafluorophosphate was dissolved in a mixed solvent (EC: DEC ═ 1:2, volume ratio) at a lithium hexafluorophosphate concentration of 1mol/L to prepare a working electrolyte.
The positive plate (active material is LiNi) of the lithium ion battery1/3Co1/3Mn1/3O2) And a negative plate metal lithium plate to form a button cell, wherein lithium trifluoroacetate lithium supplement electrolyte (marked as a button cell a) and working electrolyte (marked as a button cell b) are respectively adopted as the electrolytes, and the button cell a and the button cell b are charged to a state that the current is constant and the current is constant at 0.05 DEG to4.3V(vs Li+/Li). In the charging process, the electrochemical reaction of the positive electrode of the button cell a adopting the lithium trifluoroacetate lithium supplement electrolyte is the oxidation reaction of trifluoroacetate anions in lithium trifluoroacetate and the lithium removal reaction of a positive electrode material; the electrochemical reaction occurring at the positive electrode of button cell b using the lithium hexafluorophosphate working electrolyte is the delithiation reaction of the positive electrode material. As shown in fig. 1, the charging curves of the button cells a and b are respectively higher than that of the button cell in the prior art, and the button cells adopting the lithium supplementing electrolyte to supplement lithium all show higher positive electrode capacity performance under different electrode potentials, that is, the lithium supplementing electrolyte can supplement lithium to the negative electrode by adopting lithium trifluoroacetate. The lithium supplement amount is realized by controlling the charging voltage. As shown in FIG. 1, when the charge cut-off positive electrode potential was controlled to 3.8V, the amount of lithium supplementation was 40mAh/g in terms of positive electrode capacity, and was 22.2% of the initial charge capacity of the positive electrode material relative to 180mAh/g of positive electrode material charge capacity.
Example two:
using ternary materials (LiNi)1/3Co1/3Mn1/3O2) Hard carbon as a cathode active material and hard carbon as an anode active material are respectively used for preparing a cathode sheet and an anode sheet of the battery. Then preparing the battery core together with the diaphragm in a lamination mode, and packaging the battery core in an aluminum plastic film shell for later use.
At a certain temperature (30 ℃), dissolving lithium trifluoroacetate in a mixed solvent (EC: DEC ═ 1:2, volume ratio), wherein the concentration of lithium trifluoroacetate is 1mol/L, and preparing lithium trifluoroacetate lithium-supplement electrolyte. And dissolving lithium acetate in a mixed solvent (EC: DEC ═ 1:2, volume ratio) to obtain a lithium acetate concentration of 0.3mol/L, so as to prepare the lithium acetate lithium-supplementing electrolyte. Lithium hexafluorophosphate was dissolved in a mixed solvent (EC: DEC ═ 1:2, volume ratio) at a lithium hexafluorophosphate concentration of 1mol/L to prepare a working electrolyte.
And injecting lithium trifluoroacetate lithium supplementing electrolyte into the packaged battery cell, wherein the injection amount is 7g/Ah, after full infiltration, charging to a lithium supplementing voltage of 3.75V by adopting constant current of 0.05C, after the reaction is finished, removing the residual lithium supplementing electrolyte and gas generated by oxidation reaction, then injecting lithium hexafluorophosphate working electrolyte again, pre-charging the battery, charging to 4.2V by using a constant current of 0.1C, and discharging to 2.7V by using a constant current of 0.2C. The resulting cell was designated as cell 1.
Injecting lithium acetate lithium-supplementing electrolyte into the packaged battery cell, wherein the injection amount is 7g/Ah, after full infiltration, charging to a lithium-supplementing voltage of 3.8V by adopting a constant current of 0.05C, after reaction is completed, removing the residual lithium-supplementing electrolyte and gas generated by oxidation reaction, then injecting lithium hexafluorophosphate working electrolyte again, pre-charging the battery, charging to 4.2V by using a constant current of 0.1C, and discharging to 2.7V by using a constant current of 0.2C. The resulting cell was designated as cell 2.
For comparison, lithium hexafluorophosphate working electrolyte is injected into the packaged battery cell, and after the lithium hexafluorophosphate working electrolyte is fully soaked, the battery is directly precharged and charged to 4.2V at a constant current of 0.1C, and discharged to 2.7V at a constant current of 0.2C. The resulting cell was designated comparative cell 1.
The battery 1, the battery 2 and the comparative battery are subjected to constant volume with the battery of 0.5C and the battery of 2.7-4.2V. After constant volume, the three types of batteries are subjected to normal-temperature cycle test at a current of 1C and a voltage of 2.7-4.2V.
Example three:
the same as the second embodiment except for the following differences from the second embodiment:
and injecting lithium trifluoroacetate lithium supplementing electrolyte into the packaged battery cell, wherein the injection amount is 7g/Ah, after full infiltration, charging to a lithium supplementing voltage of 3.8V by adopting constant current of 0.02C, after the reaction is finished, removing the residual lithium supplementing electrolyte and gas generated by oxidation reaction, then injecting lithium hexafluorophosphate working electrolyte again, pre-charging the battery, charging to 4.2V by using a constant current of 0.1C, and discharging to 2.7V by using a constant current of 0.2C. The resulting cell was designated as cell 3.
Injecting lithium acetate lithium-supplementing electrolyte into the packaged battery cell, wherein the injection amount is 7g/Ah, after full infiltration, charging to a lithium-supplementing voltage of 3.85V by adopting constant current of 0.02C, after reaction is finished, removing the residual lithium-supplementing electrolyte and gas generated by oxidation reaction, then injecting lithium hexafluorophosphate working electrolyte again, pre-charging the battery, charging to 4.2V by using a constant current of 0.1C, and discharging to 2.7V by using a constant current of 0.2C. The resulting cell was designated as cell 4.
Example four:
the same as the second embodiment except for the following differences from the second embodiment:
and injecting lithium trifluoroacetate lithium supplement electrolyte (PC: DMC is 1:1, the volume ratio is 1, and the concentration of lithium trifluoroacetate is 0.5mol/L) into the packaged battery core, wherein the injection amount is 7g/Ah, after the lithium trifluoroacetate lithium supplement electrolyte is fully infiltrated, charging to a lithium supplement voltage of 3.85V by adopting constant current of 0.1C, after the reaction is finished, removing the residual lithium supplement electrolyte and gas generated by oxidation reaction, then re-injecting lithium hexafluorophosphate working electrolyte, pre-charging the battery, charging to 4.2V by using a constant current of 0.1C, and discharging to 2.7V by using a constant current of 0.2C. The resulting cell was designated as cell 5.
Injecting lithium acetate lithium-supplementing electrolyte (PC: DMC is 1:1, volume ratio, lithium acetate concentration is 1mol/L) into the packaged battery core, wherein the injection amount is 7g/Ah, after full infiltration, charging to a lithium-supplementing voltage of 3.9V by adopting a constant current of 0.1C, after reaction is completed, removing the residual lithium-supplementing electrolyte and gas generated by oxidation reaction, then re-injecting lithium hexafluorophosphate working electrolyte, pre-charging the battery, charging to 4.2V by using a constant current of 0.1C, and discharging to 2.7V by using a constant current of 0.2C. The resulting cell was designated as cell 6.
Example five:
the same as the second embodiment except for the following differences from the second embodiment:
and preparing the negative plate by taking the mixture of graphite and silicon as a negative active material.
Wherein, lithium ion batteries adopting lithium trifluoroacetate lithium supplement electrolyte and lithium acetate lithium supplement electrolyte are respectively marked as batteries 7 and 8; a lithium ion battery prepared using only the lithium hexafluorophosphate working electrolyte was designated as comparative battery 2.
Table 1 shows the performance data for the above batteries 1-6 and 7-8 compared to comparative batteries 1 and 2, respectively. The first coulombic efficiency of the lithium ion battery adopting the lithium trifluoroacetate lithium supplement electrolyte and the lithium acetate lithium supplement electrolyte is obviously higher than that of a comparative battery, the battery capacity is improved after the constant volume, and the corresponding battery energy density is improved. Fig. 2 is a normal temperature cycle chart of battery 1, battery 2 and a comparative battery, in which the capacities of battery 1 and battery 2 are higher than those of the comparative battery throughout the cycle, and the cycle lives of battery 1 and battery 2 are longer. Meanwhile, compared with the prior art, the invention has the advantages of simple process, low manufacturing cost and high safety performance, and compared with products such as CN103199217A (shown in table 1), the first coulombic efficiency of graphite or hard carbon negative battery products is also obviously improved by 1-5%.
TABLE 1
| Group of | Type (B) | First coulombic efficiency | Constant volume capacity | Capacity enhancement |
| Battery 1 | Trifluoroacetic acid lithium salt | 97％ | 14.2 | 20.3 |
| Battery | ||||
| 2 | Lithium acetate | 95％ | 13.4 | 13.6％ |
| Battery 3 | Trifluoroacetic acid lithium salt | 98％ | 14.5 | 22.9％ |
| Battery 4 | Lithium acetate | 95％ | 13.6 | 15.3％ |
| Battery 5 | Trifluoroacetic acid lithium salt | 96％ | 14.3 | 21.2 |
| Battery | ||||
| 6 | Lithium acetate | 94％ | 13.3 | 12.7％ |
| Comparative battery 1 | / | 66％ | 11.8 | — |
| Battery 7 | Trifluoroacetic acid lithium salt | 97％ | 14.6 | 14.1 |
| Battery | ||||
| 8 | Lithium acetate | 94％ | 13.9 | 8.6％ |
| |
/ | 74％ | 12.8 | — |
Claims (7)
1. A lithium supplementing method of a lithium ion battery is characterized by comprising the following steps:
(1) after the lithium ion battery is assembled and before the liquid injection process, injecting a lithium supplement electrolyte, and after the lithium supplement electrolyte fully infiltrates positive and negative pole pieces and a diaphragm inside the battery, charging the lithium ion battery to a lithium supplement voltage by using a constant lithium supplement current;
(2) removing the lithium supplement electrolyte, and injecting the working electrolyte;
wherein the lithium-supplementing electrolyte comprises an organic solution of lithium salt, and the electrode potential is 4.3V (vs Li)+below/Li), the anions of the lithium salt are unstable at the positive electrode of the lithium ion battery, an anodic oxidation reaction occurs, and a delithiation reaction of the positive electrode material occurs at the same time; wherein the lithium salt is lithium trifluoroacetate; the lithium supplementing voltage is 3.75V-4.2V.
2. The method of claim 1, wherein the concentration of the lithium salt in the organic solution of lithium salt is 0.1-1 mol/L.
3. The method of claim 1, wherein the solvent of the organic solution is one or more selected from propylene carbonate, ethylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, and methylpropyl carbonate.
4. The method of claim 2, wherein the solvent of the organic solution is one or more of propylene carbonate, ethylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate and methyl propyl carbonate.
5. The method according to any one of claims 1 to 4, wherein the amount of the lithium supplement electrolyte injected is 3g to 10 g/Ah.
6. The method for supplementing lithium according to any one of claims 1 to 4, wherein the lithium supplementing current is 0.01C to 0.2C.
7. The method according to claim 5, wherein the lithium supplementing current is 0.01C-0.2C.
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| CN113889676B (en) * | 2020-07-03 | 2023-06-20 | 北京好风光储能技术有限公司 | Repairing and regenerating method for lithium-containing battery |
| CN112599723A (en) | 2020-12-03 | 2021-04-02 | 天津市捷威动力工业有限公司 | Lithium-supplement negative pole piece, preparation method thereof and lithium ion battery |
| CN113097567B (en) * | 2021-03-29 | 2022-04-12 | 湖南高远电池有限公司 | Manufacturing method of high-energy-density soft package battery |
| CN113078364A (en) * | 2021-03-29 | 2021-07-06 | 中南大学 | Manufacturing method of high-energy-density aluminum-shell lithium ion battery |
| CN114243131A (en) * | 2021-12-23 | 2022-03-25 | 湖北亿纬动力有限公司 | Lithium supplementing method and lithium ion battery thereof |
| CN114744190B (en) * | 2022-03-22 | 2024-06-11 | 浙江南都电源动力股份有限公司 | Additive for preventing excessive lithium supplement of pre-lithiated cathode and method thereof and lithium ion battery |
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| TW201611377A (en) * | 2014-06-12 | 2016-03-16 | 安普雷斯公司 | Prelithiation solutions for lithium-ion batteries |
| CN104681311A (en) * | 2014-12-12 | 2015-06-03 | 宁波南车新能源科技有限公司 | Novel lithium pre-embedding method of lithium ion capacitor |
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