CN108878974A - A kind of lithium ion battery mends lithium electrolyte and mends lithium method - Google Patents
A kind of lithium ion battery mends lithium electrolyte and mends lithium method Download PDFInfo
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- CN108878974A CN108878974A CN201710343164.8A CN201710343164A CN108878974A CN 108878974 A CN108878974 A CN 108878974A CN 201710343164 A CN201710343164 A CN 201710343164A CN 108878974 A CN108878974 A CN 108878974A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0568—Liquid materials characterised by the solutes
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention provides a kind of lithium ion battery and mends lithium electrolyte and mend lithium method.First, the benefit lithium electrolyte includes organic solvent and lithium salts, electrode potential 4.3V (vs Li+/Li) below when, the anion of lithium salts is unstable in lithium ion cell positive, anodic oxidation decomposition reaction can occur, the insertion reaction of lithium ion occurs for corresponding cathode.The benefit lithium method includes step:It will mend in lithium electrolyte injection lithium ion battery, and by pre-charging lithium ion batteries to lithium voltage is mended, mend lithium amount cathode is mended lithium and be controlled, lithium to be mended is after the reaction was completed, remaining benefit lithium electrolyte is removed, conventional electrolysis liquid is refilled, preliminary filling formation process then is carried out to battery.Operation of the present invention is simple, it is not necessary that existing producing line is transformed, it is only necessary to and it is appropriate to change battery preliminary filling technique, benefit lithium accurate, uniformly can be carried out to cathode, so as to improve the coulombic efficiency for the first time of battery, improve energy density, improve cycle performance.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of lithium ion battery mends lithium electrolyte and mends lithium side
Method.
Background technique
Commercial lithium-ion batteries generally use the materials such as graphite, hard carbon or the alloy for capableing of reversible deintercalate lithium ions at present
As negative electrode material, during lithium ion battery initial charge, the solid electrolyte interface film of negative electrode material Surface Creation
(SEI film) and some side reactions consume lithium ion of a part in positive electrode, irreversible capacity are formed, to lead
The coulombic efficiency for the first time and capacity for sending a telegraph core reduce.
It has been investigated that the lithium ion consumed can be supplemented by mending lithium (or making pre- embedding lithium) technology,
To promote the first charge discharge efficiency and energy density of lithium ion battery.For example, Publication No. CN104993098A,
The patent application of CN102779975A and CN103199217A discloses the technical side that lithium source is introduced in lithium ion battery
Case.Its main contents is to be mixed SLMP lithium metal powder with cathode by slurry, calendering or paint-on technique, or by metal lithium sheet
It is covered on negative electrode tab surface and carries out pre- embedding lithium.However, in the above technical know-how benefit lithium can be carried out to battery core, but in reality
When putting into industrial production, many technological problems are faced:Production technology is complicated, and operating environment is harsh, needs to carry out production line
Partially, even comprehensively transformation or superseded, so that manufacturing cost significantly improves and have the discarded waste of production equipment.Together
When, it is uneven due to being difficult to control pre- lithium-inserting amount, embedding lithium, it is poor so as to cause battery core consistency, and occur analysing lithium, cycle performance declines
Subtract the problems such as serious.Also, due to the mode of its " macroscopic view " embedding lithium, since it is difficult to control lithium-inserting amount, it has to increase embedding lithium
Range and dosage, also effectively caused the waste of material, cost it is further up, the lithium of extra addition, which can not recycle, to be made
With unfortunately.
In view of this, it is necessory to provide it is a kind of it is easy to operate, prior art equipment is influenced low, dosage save rationally,
The high technology of production homogeneity of product realizes the promotion of lithium ion battery coulombic efficiency and capacity for the first time.
Summary of the invention
Lithium electrolyte is mended the purpose of the present invention is to provide a kind of lithium ion battery and mends lithium method, it is electric by using lithium is mended
Solution liquid come realize it is controllable to negative electrode of lithium ion battery, uniformly mend lithium, simplify production technology, to effectively supplement lithium-ion electric
The irreversible capacity loss in pond improves lithium ion battery coulombic efficiency, cycle performance and energy density for the first time.
In order to achieve the above object, the present invention adopts the following technical scheme that:
A kind of lithium ion battery benefit lithium electrolyte, the organic solution including lithium salts;The electrode of the lithium ion cell positive
Current potential 4.3V (vs Li+/Li) below when, the anion of the lithium salts is unstable in lithium ion cell positive, it may occur that anode
Oxidation reaction generates the by-product of predominantly gas;In this voltage range, de- lithium reaction can also occur simultaneously for positive electrode.
When the anodic oxidation reactions of the lithium salts anion occur simultaneously for anode and positive electrode takes off lithium reaction, the lithium of the lithium salts from
In cathode embedding lithium reaction occurs for son.The total result of above-mentioned reaction achievees the effect that carry out mending lithium to cathode, in this technology side
It is known as mending lithium reaction in case.Meanwhile the present invention also provides a kind of lithium ion batteries to mend lithium method, the method comprising the steps of:It will mend
After lithium electrolyte injection encapsulation in the lithium ion battery of (battery after the assembly is completed, before conventional fluid injection process), lithium electrolysis to be mended
After liquid sufficiently infiltrates inside battery positive/negative plate and diaphragm, completed using constant current charging to lithium voltage, lithium reaction to be mended is mended
Afterwards, residue is mended lithium electrolyte to remove, injects conventional Working electrolyte, the subsequent routines such as preliminary filling chemical conversion then are carried out to battery
Process.
Wherein, the present invention in so-called " Working electrolyte " be this field lithium ion battery in can be any kind conventional use of
The electrolyte of class.Wherein, the step of sufficiently infiltrating is identical as conventional electrolysis liquid immersion step, preferably infiltration 24-48h.
Wherein, the lithium salts is trifluoroacetic acid lithium or lithium acetate;Lithium salt is 0.1-1mol/L, for lithium salts solubility
It can suitably be adjusted by adjusting experimental temperature, temperature range is 25 DEG C~60 DEG C.The solvent of the organic solution is carbonic acid third
Enester (PC), ethylene carbonate (EC), butylene (BC), dimethyl carbonate (DMC), diethyl carbonate (DEC), carbonic acid first
One or more of propyl ester (MPC).And, it is preferred that solvent as far as possible with it is contained in the routine work electrolyte that then uses
Solvent is identical.
Wherein, the reservoir quantity for mending lithium electrolyte is 3g-10g/Ah, and the size for mending lithium electric current is 0.01C-0.2C, is mended
Lithium voltage is 3.75V-4.2V.Mending lithium amount can be by mending lithium salt in lithium electrolyte, the reservoir quantity for mending lithium electrolyte, mending lithium
It electric current and mends lithium voltage and controls, adjusts, achieve the purpose that accurately to mend lithium with this.
And the benefit lithium demand of negative electrode of lithium ion battery should be adjusted according to the difference of lithium ion battery positive and negative electrode material
Whole, for graphite negative electrodes, benefit lithium amount is between the 1%~30% of battery design capacity, and for hard carbon class cathode, mending lithium amount is
Between the 10%~40% of battery design capacity, alloy type cathode lower for efficiency, mending lithium amount is battery design capacity
Between 10%~50%.
Tradition can be overcome to mend lithium technology bring obstacle with technical solution provided by the invention, solution cost is excessively high, ring
The problems such as border requires harshness, and safety is poor.Meanwhile, it is capable to lithium-inserting amount and embedding lithium uniformity be accurately controlled, to reduce lithium
The irreversible capacity of ion battery, the effective coulombic efficiency for the first time for improving battery, cycle life improve its energy density, protect
Demonstrate,proving battery has better chemical property and safety.Lithium ion battery is prepared with method provided by the invention simultaneously,
It is easy to operate, without being transformed to existing production line, it is only necessary to appropriate adjustment is carried out to preliminary filling technique, it is low in cost.Also, essence
Really for the accurate supply of lithium demand offer is mended, the waste of material and the issuable other problems of excess stock are avoided.Meanwhile
After the benefit lithium electrolyte of recycling carries out respective handling, it still can be recycled, be theoretically obtainable having for lithium salts utilization rate 100%
Beneficial effect.
Detailed description of the invention
Fig. 1 is the charging curve using button cell a, b made of method (embodiment one) of the invention.
Fig. 2 is the lithium ion battery room temperature cyclic curve using moving party's method of the present invention preparation.
Specific embodiment
Lithium electrolyte is mended to lithium ion battery of the invention combined with specific embodiments below and corresponding lithium method of mending is done more in detail
Most description.But the present invention is not limited to following embodiments.
Embodiment one:
Trifluoroacetic acid lithium is dissolved in the mixed solvent (EC by (30 DEG C) at a certain temperature:DEC=1:2, volume ratio), three
Fluoroacetic acid lithium concentration is 1mol/L, is configured to trifluoroacetic acid lithium and mends lithium electrolyte.Lithium hexafluoro phosphate is dissolved in the mixed solvent
(EC:DEC=1:2, volume ratio), hexafluorophosphoric acid lithium concentration is 1mol/L, is configured to Working electrolyte.
By based lithium-ion battery positive plate (active material LiNi1/3Co1/3Mn1/3O2) and negative electrode tab metal lithium sheet composition button
Formula battery, electrolyte are respectively adopted trifluoroacetic acid lithium benefit lithium electrolyte and (are denoted as button cell a) and Working electrolyte (is denoted as button
Battery b), by button cell a and button cell b 0.05C electric current constant-current charge to 4.3V (vs Li+/Li).It recharged here
Cheng Zhong is in trifluoroacetic acid lithium using the electrochemical reaction that the anode that trifluoroacetic acid lithium mends the button cell a of lithium electrolyte occurs
The oxidation reaction of trifluoroacetic acid root anion and the de- lithium reaction of positive electrode;Using the button of lithium hexafluoro phosphate Working electrolyte
The electrochemical reaction that the anode of battery b occurs is the de- lithium reaction of positive electrode.The charging curve of above-mentioned button cell a, b are as schemed
Shown in 1, under Different electrodes current potential, higher positive electrode capacity is shown using the button cell that benefit lithium electrolyte mend lithium
It plays, that is, mending lithium electrolyte using trifluoroacetic acid lithium may be implemented the benefit lithium to cathode.Mend lithium amount by control charging voltage come
It realizes.Such as Fig. 1, if controlling charge cutoff anodic potentials in 3.8V, mending lithium amount to be scaled positive electrode capacity and play is 40mAh/
G mends 22.2% that lithium amount is positive electrode initial charge capacity relative to positive electrode charging capacity 180mAh/g.
Embodiment two:
With ternary material (LiNi1/3Co1/3Mn1/3O2) positive electrode active materials are used as, hard carbon divides as negative electrode active material
Positive and negative plate not to prepare battery.Then together with diaphragm, battery core is prepared into using lamination process, is packaged in plastic-aluminum putamina
In body, for use.
Trifluoroacetic acid lithium is dissolved in the mixed solvent (EC by (30 DEG C) at a certain temperature:DEC=1:2, volume ratio), three
Fluoroacetic acid lithium concentration is 1mol/L, is configured to trifluoroacetic acid lithium and mends lithium electrolyte.Lithium acetate is dissolved in the mixed solvent (EC:DEC
=1:2, volume ratio), acetic acid lithium concentration is 0.3mol/L, is configured to lithium acetate and mends lithium electrolyte.Lithium hexafluoro phosphate is dissolved in mixed
(EC in bonding solvent:DEC=1:2, volume ratio), hexafluorophosphoric acid lithium concentration is 1mol/L, is configured to Working electrolyte.
Trifluoroacetic acid lithium is mended in the battery core after lithium electrolyte injection encapsulation, reservoir quantity 7g/Ah, after sufficiently infiltrating,
It is charged to using constant current 0.05C and mends lithium voltage 3.75V, it is anti-to after the reaction was completed, remove remaining benefit lithium electrolyte and oxidation
Then the gas that should be generated refills lithium hexafluoro phosphate Working electrolyte, carry out preliminary filling chemical conversion to battery, filled with 0.1C constant current
Electricity is to 4.2V, 0.2C constant-current discharge to 2.7V.Gained battery is denoted as battery 1.
Lithium acetate is mended in the battery core after lithium electrolyte injection encapsulation, reservoir quantity 7g/Ah is used after sufficiently infiltrating
Constant current 0.05C, which is charged to, mends lithium voltage 3.8V, generates to after the reaction was completed, remove remaining benefit lithium electrolyte and oxidation reaction
Gas, then refill lithium hexafluoro phosphate Working electrolyte, to battery carry out preliminary filling chemical conversion, extremely with 0.1C constant-current charge
4.2V, 0.2C constant-current discharge are to 2.7V.Gained battery is denoted as battery 2.
As a comparison, directly right after sufficiently infiltrating in the battery core after the injection of lithium hexafluoro phosphate Working electrolyte being encapsulated
Battery carries out preliminary filling chemical conversion, with 0.1C constant-current charge to 4.2V, 0.2C constant-current discharge to 2.7V.Gained battery is denoted as control cell
1。
By battery 1, battery 2 and control cell carry out constant volume between 2.7~4.2V with 0.5C battery.After constant volume, by three classes
Battery carries out normal temperature circulation test with 1C electric current between 2.7~4.2V.
Embodiment three:
With embodiment two, except the difference below with embodiment two:
Trifluoroacetic acid lithium is mended in the battery core after lithium electrolyte injection encapsulation, reservoir quantity 7g/Ah, after sufficiently infiltrating,
It is charged to using constant current 0.02C and mends lithium voltage 3.8V, to after the reaction was completed, remove remaining benefit lithium electrolyte and oxidation reaction
Then the gas of generation refills lithium hexafluoro phosphate Working electrolyte, preliminary filling chemical conversion is carried out to battery, with 0.1C constant-current charge
To 4.2V, 0.2C constant-current discharge to 2.7V.Gained battery is denoted as battery 3.
Lithium acetate is mended in the battery core after lithium electrolyte injection encapsulation, reservoir quantity 7g/Ah is used after sufficiently infiltrating
Constant current 0.02C, which is charged to, mends lithium voltage 3.85V, raw to after the reaction was completed, remove remaining benefit lithium electrolyte and oxidation reaction
At gas, then refill lithium hexafluoro phosphate Working electrolyte, to battery carry out preliminary filling chemical conversion, extremely with 0.1C constant-current charge
4.2V, 0.2C constant-current discharge are to 2.7V.Gained battery is denoted as battery 4.
Example IV:
With embodiment two, except the difference below with embodiment two:
Trifluoroacetic acid lithium is mended into lithium electrolyte (PC:DMC=1:1, volume ratio, trifluoroacetic acid lithium concentration is 0.5mol/L) note
In battery core after entering encapsulation, reservoir quantity 7g/Ah is charged to using constant current 0.1C after sufficiently infiltrating and is mended lithium voltage
Then 3.85V refills hexafluoro phosphorus to after the reaction was completed, remove the remaining gas mending lithium electrolyte and oxidation reaction and generating
Sour lithium Working electrolyte carries out preliminary filling chemical conversion to battery, with 0.1C constant-current charge to 4.2V, 0.2C constant-current discharge to 2.7V.Institute
It obtains battery and is denoted as battery 5.
Lithium acetate is mended into lithium electrolyte (PC:DMC=1:1, volume ratio, after acetic acid lithium concentration is 1mol/L) injection encapsulation
In battery core, reservoir quantity 7g/Ah is charged to using constant current 0.1C after sufficiently infiltrating and is mended lithium voltage 3.9V, wait react
Cheng Hou removes the remaining gas mending lithium electrolyte and oxidation reaction and generating, then refills lithium hexafluoro phosphate Working electrolyte,
Preliminary filling chemical conversion is carried out to battery, with 0.1C constant-current charge to 4.2V, 0.2C constant-current discharge to 2.7V.Gained battery is denoted as battery 6.
Embodiment five:
With embodiment two, except the difference below with embodiment two:
Using the mixture of graphite and silicon as negative electrode active material, to prepare negative electrode tab.
Wherein, electricity is denoted as using the lithium ion battery that trifluoroacetic acid lithium mends lithium electrolyte and lithium acetate benefit lithium electrolyte respectively
Pond 7 and 8;Control cell 2 is denoted as using only lithium ion battery prepared by lithium hexafluoro phosphate Working electrolyte.
Table 1 show above-mentioned battery 1-6 and 7-8 and compares respectively with the performance data of control cell 1 and 2.Using trifluoro second
The coulombic efficiency for the first time that sour lithium mends the lithium ion battery of lithium electrolyte and lithium acetate benefit lithium electrolyte is significantly higher than control cell, fixed
Battery capacity improves after appearance, and respective battery energy density is improved.Fig. 2 is that the room temperature of battery 1, battery 2 and control cell follows
Ring figure, in entire cyclic process, the capacity of battery 1 and battery 2 is above control cell, the cycle life of battery 1 and battery 2
It is longer.Meanwhile compared with prior art, the present invention is other than simple process, cheap, security performance are high, and such as
The product of CN103199217A compares (e.g., shown in table 1), the coulombic efficiency for the first time of graphite or hard carbon class negative battery product
There is significantly improving for 1%-5%.
Table 1
Group | Type | Coulombic efficiency for the first time | Constant volume capacity | Capacity improves |
Battery 1 | Trifluoroacetic acid lithium | 97% | 14.2 | 20.3% |
Battery 2 | Lithium acetate | 95% | 13.4 | 13.6% |
Battery 3 | Trifluoroacetic acid lithium | 98% | 14.5 | 22.9% |
Battery 4 | Lithium acetate | 95% | 13.6 | 15.3% |
Battery 5 | Trifluoroacetic acid lithium | 96% | 14.3 | 21.2% |
Battery 6 | Lithium acetate | 94% | 13.3 | 12.7% |
Control cell 1 | / | 66% | 11.8 | — |
Battery 7 | Trifluoroacetic acid lithium | 97% | 14.6 | 14.1% |
Battery 8 | Lithium acetate | 94% | 13.9 | 8.6% |
Control cell 2 | / | 74% | 12.8 | — |
Claims (10)
1. a kind of benefit lithium electrolyte of lithium ion battery, which is characterized in that the benefit lithium electrolyte includes the organic solution of lithium salts, electricity
Electrode potential 4.3V (vs Li+/Li) below when, the anion of the lithium salts is unstable in lithium ion cell positive, occur anode
Oxidation reaction, while the de- lithium reaction of positive electrode occurs.
2. a kind of benefit lithium electrolyte of lithium ion battery according to claim 1, which is characterized in that the lithium salts is trifluoro
Lithium acetate or lithium acetate.
3. a kind of benefit lithium electrolyte of lithium ion battery according to claim 1 or 2, which is characterized in that the lithium salts has
The concentration of lithium salts is 0.1-1mol/L in machine solution.
4. a kind of benefit lithium electrolyte of lithium ion battery according to claim 1 to 3, which is characterized in that described organic
The solvent of solution is propene carbonate (PC), ethylene carbonate (EC), butylene (BC), dimethyl carbonate (DMC), carbonic acid
One or more of diethylester (DEC), methyl propyl carbonate (MPC).
5. a kind of benefit lithium electrolyte of lithium ion battery according to any of the above-described claim, which is characterized in that lithium from
Before the step of injection Working electrolyte in sub- cell manufacturing process, by injecting the benefit lithium electrolyte, by lithium ion battery
It is charged to constant benefit lithium electric current and mends lithium voltage, to realize the benefit lithium of lithium ion battery.
6. a kind of benefit lithium method of lithium ion battery, which is characterized in that the described method comprises the following steps:
(1) lithium ion battery after the assembly is completed, before fluid injection process, lithium electrolyte is mended in injection, and the benefit lithium electrolyte is abundant
After infiltrating inside battery positive/negative plate and diaphragm, lithium ion battery is charged to constant benefit lithium electric current and mends lithium voltage;
(2) lithium electrolyte will be mended to remove, and will inject Working electrolyte;
Wherein, the lithium electrolyte of mending is according to any benefit lithium electrolyte of claim 1-4.
7. a kind of benefit lithium method of lithium ion battery according to claim 6, which is characterized in that the benefit lithium electrolyte
Reservoir quantity is 3g-10g/Ah.
8. a kind of benefit lithium method of lithium ion battery according to claim 6, which is characterized in that the benefit lithium electric current is
0.01C-0.2C。
9. a kind of benefit lithium method of lithium ion battery according to claim 6, which is characterized in that the benefit lithium voltage is
3.75V-4.2V。
10. a kind of lithium ion battery, which is characterized in that the lithium ion battery utilizes any benefit lithium of claim 1-5
Electrolyte is made or the preparation method of the lithium ion battery includes according to any benefit lithium method of claim 6-9.
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CN113889676A (en) * | 2020-07-03 | 2022-01-04 | 北京好风光储能技术有限公司 | Repairing and regenerating method for lithium-containing battery |
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CN113078364A (en) * | 2021-03-29 | 2021-07-06 | 中南大学 | Manufacturing method of high-energy-density aluminum-shell lithium ion battery |
CN113097567A (en) * | 2021-03-29 | 2021-07-09 | 湖南高远电池有限公司 | Manufacturing method of high-energy-density soft package 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 |
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 |
CN114744190A (en) * | 2022-03-22 | 2022-07-12 | 浙江南都电源动力股份有限公司 | Additive for preventing partial lithium supplement excess of pre-lithiation negative electrode, method thereof and lithium ion battery |
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 |
CN117728038A (en) * | 2023-08-08 | 2024-03-19 | 荣耀终端有限公司 | Preparation method and system of lithium battery |
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