CN107565096A - A kind of anode plate for lithium ionic cell and its processing method and a kind of lithium ion battery - Google Patents
A kind of anode plate for lithium ionic cell and its processing method and a kind of lithium ion battery Download PDFInfo
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Abstract
The invention discloses a kind of anode plate for lithium ionic cell and its processing method and a kind of lithium ion battery, the processing method of anode plate for lithium ionic cell of the present invention is to be pre-processed anode plate for lithium ionic cell before winding, anode plate for lithium ionic cell surface is set to previously generate one layer of SEI film, the anode plate for lithium ionic cell being prepared according to the processing method is provided simultaneously, and provides the lithium ion battery comprising the anode plate for lithium ionic cell.The present invention forms one layer of SEI film by elder generation on negative plate, then carry out with positive plate being assembled into battery again, avoid and the battery reversible capacity loss so as to caused by by preliminary filling formation SEI films again is first formed in traditional approach, reduce the waste of material, the consumption of high-purity lithium is saved, battery cost is reduced, and reduces battery initial charge capacitance loss, so as to improve battery capacity.
Description
Technical field
The present invention relates to cell art, particularly relates to a kind of anode plate for lithium ionic cell and its processing method and one kind
Lithium ion battery.
Background technology
Lithium ion battery has the characteristics that high energy density, environmental protection, memory-less effect, is widely used to industry-by-industry,
But every field is in battery capacity requirement more and more higher, particularly portable machine.Generally, in lithium ion battery charge and discharge first
In electric process, electrode material reacts with electrolyte on solid-liquid phase interface, forms one layer and is covered in electrode material surface
Passivation layer.This passivation layer is a kind of boundary layer, has the feature of solid electrolyte, is that electronic body is Li+It is excellent
Conductor, Li+The passivation layer freely insertion can be passed through and deviate from, therefore this layer of passivating film is referred to as " solid electrolyte interface
Film ", abbreviation SEI films.The formation of SEI films consumes part lithium ion, causes after a part of elemental lithium is embedded into negative pole in positive pole
The compound of lithium is formed, this process is irreversible, causes a part of capacity irreversible loss, so as to cause the capacity attenuation of lithium battery
Become apparent from the reduction of cycle efficieny, especially cycle efficieny reduction first.
Chinese patent CN101777641A, which discloses a kind of lithium battery cathode plate and preparation method, improves graphite cathode piece
Structure, security performance is enhanced, but be confined to graphite material as negative pole, without fundamentally solving the capacity of negative material
Problem.Chinese patent CN102315425A discloses a kind of preparation method of lithium battery cathode plate, and graphite cathode has been carried out not
Same arrangement is still confined to graphite material as negative pole so as to save material, can not solve graphite material as negative pole
Capacity limitation problem.Document《Osaka titanium industry science and technology production high-performance lithium cell negative electrode material SiO》(inorganic chemicals industry,
Inorganic Chemicals Industry, 2013) test performance of the silicon based anode material relative to graphite cathode material
Optimization, but actual production is not applied to, still in laboratory theory stage.Document《Lithium ion battery silicon cathode material declines
Move back the progress of mechanism》The performance that (Ma Zengsheng, Zhou Yichun, Liu Jun, Proceedings of Mechanics, 2013) has focused on silicon based anode material is ground
Study carefully, theoretically predict the degeneration benefit of silicon based anode material, while also affirmed the superiority of silicon based anode material, still
The experience for being applied to actual production does not have but.Chinese patent CN101228652A discloses a kind of lithium rechargeable battery and used
Negative pole, its manufacture method and the lithium rechargeable battery using the negative pole, it is proposed that negative pole silicon substrate pole piece is in first discharge and recharge
After can aoxidize lithium is deposited on layer so as to cause to crack, therefore employ, but do not have for battery capacity and cycle performance
Too big improvement.
The content of the invention
In view of this, it is an object of the invention to propose a kind of anode plate for lithium ionic cell and its processing method and a kind of lithium
Negative plate is pre-processed, negative pole is produced one layer of SEI film in advance, avoid positive pole by ion battery, the present invention before winding
Capacity irreversible loss.
Based on above-mentioned purpose, a kind of processing method of anode plate for lithium ionic cell provided by the invention, by lithium ion battery
Negative plate is pre-processed before winding, anode plate for lithium ionic cell surface is previously generated one layer of SEI film.
In the present invention, it is preferred to, anode plate for lithium ionic cell is put into electrolyte, enters line precharge, charging current
For 0.01~0.05C, the charging interval is 2~6 hours, is shelved 4~6 minutes, then anode plate for lithium ionic cell is discharged into 0.2V,
Placed 4~6 hours under vacuum, until after anode plate for lithium ionic cell dry tack free.
In the present invention, it is preferred to, the anode plate for lithium ionic cell is graphite cathode piece, and the electrolyte is hexafluoro phosphorus
Sour lithium electrolyte.
The present invention pre-processes before winding to negative plate, negative plate surface is previously generated one layer of SEI film, specific step
Suddenly it is：In the case where drying vacuum, graphite cathode piece is put into electrolyte (1mol/L lithium hexafluoro phosphate organic solution), carried out pre-
Charging, charging current are about 0.01C~0.05C, and the charging interval is 2~6 hours, is shelved 5 minutes, then negative plate is discharged into
0.2V (relative standard's hydrogen potential), place 5 hours under vacuum, until winding, fluid injection, sealing, chemical conversion divide after pole piece is dried
Hold.
Further, the present invention has been also provided to a kind of anode plate for lithium ionic cell, is born according to described lithium ion battery
The processing method of pole piece is prepared.
On the other hand, present invention also offers a kind of lithium ion battery, including described anode plate for lithium ionic cell.Using
The lithium ion battery that the surface of the present invention previously generates the graphite cathode piece composition of one layer of SEI film has high power capacity.
In the present invention, it is preferred to, in addition to casing of lithium ion battery, the casing of lithium ion battery is interior to be provided with by positive pole
Piece, surface previously generate the negative plate of one layer of SEI film and the pole piece of barrier film composition, and electrolysis is injected in casing of lithium ion battery
Liquid, the electrolyte are lithium hexafluorophosphate electrolyte solution.
In the present invention, it is preferred to, the positive plate is lithium cobaltate cathode piece, and the electrolyte is electrolysed for lithium hexafluoro phosphate
Liquid, the barrier film are cegard23 barrier films.
Compared with prior art, the beneficial effects of the present invention are：
(1) present invention forms one layer of SEI film by elder generation on negative plate, then carries out with positive plate being assembled into battery again,
Avoid and the battery reversible capacity loss so as to caused by by preliminary filling formation SEI films again is first formed in traditional approach, reduce material
The waste of material, the consumption of high-purity lithium is saved, reduced battery cost；And battery initial charge capacitance loss is reduced, so as to
Improve battery capacity.
(2) processing method of anode plate for lithium ionic cell of the present invention is implemented simple, it is easy to accomplish, it can be transported completely with scale
Industrialized production for lithium ion battery.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with specific embodiment, to this hair
Bright further description.
The preparation method for the lithium hexafluoro phosphate organic liquor that following examples are related to：Lithium halide after drying and dehydrating is dissolved
It is then closed to be passed through quantitative phosphorus pentafluoride gas in anhydrous hydrogen fluoride；Temperature be -15~60 DEG C, pressure be 0~
Reacted under the conditions of 0.4MPa, the lithium hexafluorophosphate solution of 20% or so concentration is made, after the drying of inert gas thermal current
To lithium hexafluoro phosphate powdered crystalline；The six of electrolyte requirement are obtained by the drying of inert gas thermal current and vacuum drying again
Lithium fluophosphate electrolyte；By hexafluorophosphoric acid lithium electrolyte and LITHIUM BATTERY organic carbonate solvents mixed dissolution, pass through accurate mistake
Filter, obtains lithium ion battery 1mol/L lithium hexafluorophosphate electrolyte solution.
Embodiment 1
(1) preparation of graphite cathode piece
Negative pole uses Bei Terui native graphites, by native graphite and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain graphite cathode piece；
(2) pretreatment of graphite cathode piece
Graphite cathode piece is put into electrolyte (1mol/L lithium hexafluoro phosphate organic solution), enters line precharge, is charged
Electric current is 0.02C, and the charging interval is 2 hours, is shelved 5 minutes, then graphite cathode piece is discharged into 0.2V (relative standard's hydrogen electricity
Gesture), place 5 hours under vacuum, until after graphite cathode piece dry tack free, obtain to surface and previously generate the graphite of one layer of SEI film
Negative plate；
(3) preparation of lithium cobaltate cathode piece
Positive pole uses the auspicious auspicious cobalt acid lithium in Changsha, by cobalt acid lithium and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain lithium cobaltate cathode piece；
(4) preparation of lithium ion battery
The graphite cathode piece that pole piece is previously generated to one layer of SEI film according to positive plate, barrier film and surface sequentially uses successively
Takeup type is assembled into Battery Pole Core, and the barrier film uses cegard23 barrier films, Battery Pole Core is put into casing of lithium ion battery,
Injecting electrolyte, electrolyte makes square 900mah batteries using self-control 1mol/L lithium hexafluoro phosphate organic liquor, 5 × 34 ×
50mm, after completing sealing, 45 DEG C are toasted 3 days.0.02C is charged to 4.1V by 0.2C discharges into 3.0V.
Embodiment 2
(1) preparation of graphite cathode piece
Negative pole uses Bei Terui native graphites, by native graphite and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain graphite cathode piece；
(2) pretreatment of graphite cathode piece
Graphite cathode piece is put into electrolyte (1mol/L lithium hexafluoro phosphate organic solution), enters line precharge, is charged
Electric current is 0.02C, and the charging interval is 3 hours, is shelved 5 minutes, then graphite cathode piece is discharged into 0.2V (relative standard's hydrogen electricity
Gesture), place 5 hours under vacuum, until after graphite cathode piece dry tack free, obtain to surface and previously generate the graphite of one layer of SEI film
Negative plate；
(3) preparation of lithium cobaltate cathode piece
Positive pole uses the auspicious auspicious cobalt acid lithium in Changsha, by cobalt acid lithium and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain lithium cobaltate cathode piece；
(4) preparation of lithium ion battery
The graphite cathode piece that pole piece is previously generated to one layer of SEI film according to positive plate, barrier film and surface sequentially uses successively
Takeup type is assembled into Battery Pole Core, and the barrier film uses cegard23 barrier films, Battery Pole Core is put into casing of lithium ion battery,
Injecting electrolyte, electrolyte makes square 900mah batteries using self-control 1mol/L lithium hexafluoro phosphate organic liquor, 5 × 34 ×
50mm, after completing sealing, 45 DEG C are toasted 3 days.0.02C is charged to 4.1V by 0.2C discharges into 3.0V.
Embodiment 3
(1) preparation of graphite cathode piece
Negative pole uses Bei Terui native graphites, by native graphite and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain graphite cathode piece；
(2) pretreatment of graphite cathode piece
Graphite cathode piece is put into electrolyte (1mol/L lithium hexafluoro phosphate organic solution), enters line precharge, is charged
Electric current is 0.02C, and the charging interval is 4 hours, is shelved 5 minutes, then graphite cathode piece is discharged into 0.2V (relative standard's hydrogen electricity
Gesture), place 5 hours under vacuum, until after graphite cathode piece dry tack free, obtain to surface and previously generate the graphite of one layer of SEI film
Negative plate；
(3) preparation of lithium cobaltate cathode piece
Positive pole uses the auspicious auspicious cobalt acid lithium in Changsha, by cobalt acid lithium and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain lithium cobaltate cathode piece；
(4) preparation of lithium ion battery
The graphite cathode piece that pole piece is previously generated to one layer of SEI film according to positive plate, barrier film and surface sequentially uses successively
Takeup type is assembled into Battery Pole Core, and the barrier film uses cegard23 barrier films, Battery Pole Core is put into casing of lithium ion battery,
Injecting electrolyte, electrolyte makes square 900mah batteries using self-control 1mol/L lithium hexafluoro phosphate organic liquor, 5 × 34 ×
50mm, after completing sealing, 45 DEG C are toasted 3 days.0.02C is charged to 4.1V by 0.2C discharges into 3.0V.
Embodiment 4
(1) preparation of graphite cathode piece
Negative pole uses Bei Terui native graphites, by native graphite and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain graphite cathode piece；
(2) pretreatment of graphite cathode piece
Graphite cathode piece is put into electrolyte (1mol/L lithium hexafluoro phosphate organic solution), enters line precharge, is charged
Electric current is 0.04C, and the charging interval is 2 hours, is shelved 5 minutes, then graphite cathode piece is discharged into 0.2V (relative standard's hydrogen electricity
Gesture), place 5 hours under vacuum, until after graphite cathode piece dry tack free, obtain to surface and previously generate the graphite of one layer of SEI film
Negative plate；
(3) preparation of lithium cobaltate cathode piece
Positive pole uses the auspicious auspicious cobalt acid lithium in Changsha, by cobalt acid lithium and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain lithium cobaltate cathode piece；
(4) preparation of lithium ion battery
The graphite cathode piece that pole piece is previously generated to one layer of SEI film according to positive plate, barrier film and surface sequentially uses successively
Takeup type is assembled into Battery Pole Core, and the barrier film uses cegard23 barrier films, Battery Pole Core is put into casing of lithium ion battery,
Injecting electrolyte, electrolyte makes square 900mah batteries using self-control 1mol/L lithium hexafluoro phosphate organic liquor, 5 × 34 ×
50mm, after completing sealing, 45 DEG C are toasted 3 days.0.02C is charged to 4.1V by 0.2C discharges into 3.0V.
Comparative example 1
The difference of this comparative example and embodiment 1 is that graphite cathode piece does not pre-process, and concretely comprises the following steps：
(1) preparation of graphite cathode piece
Negative pole uses Bei Terui native graphites, by native graphite and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain graphite cathode piece；
(2) preparation of lithium cobaltate cathode piece
Positive pole uses the auspicious auspicious cobalt acid lithium in Changsha, by cobalt acid lithium and Kynoar (PVDF), N-methyl pyrrolidones
Etc. (NMP) it is mixed evenly, coated on obtained aluminium foil, the coating thickness of cobalt acid lithium is 20~100 μm, coated face density
For 40~100g/m2, dried dry with 90~120 DEG C in an oven, roll-in, roll-in are then carried out with 12~13MPa pressure
Density domination is in 1.2~1.7g/cm3, section, obtain lithium cobaltate cathode piece；
(3) preparation of lithium ion battery
The graphite cathode piece that pole piece is previously generated to one layer of SEI film according to positive plate, barrier film and surface sequentially uses successively
Takeup type is assembled into Battery Pole Core, and the barrier film uses cegard23 barrier films, Battery Pole Core is put into casing of lithium ion battery,
Injecting electrolyte, electrolyte makes square 900mah batteries using self-control 1mol/L lithium hexafluoro phosphate organic liquor, 5 × 34 ×
50mm, after completing sealing, 45 DEG C are toasted 3 days.0.02C is charged to 4.1V by 0.2C discharges into 3.0V.
Volume test is carried out to embodiment 1-4 and comparative example 1 lithium ion battery prepared, method of testing is：(1) test electricity
Pond 0.5C capacity；(2) battery 0.2C is fully charged, 50C discharges into 2.0V, records discharge capacity；(3) battery normal temperature 0.2C is filled
Full electric, after shelving 4 hours at -20 DEG C, 2C discharges into 2.0V, records discharge capacity.Obtained data are as shown in table 1.
Table 1
According to table 1 as can be seen that the 0.5C capacity of lithium ion battery prepared by embodiment 1-4 is compared with lithium prepared by comparative example 1
Ion battery, which adds more than 1.5%, 0.2C discharge capacities and adds more than 2.6%, 0.2C discharge capacities (- 20 DEG C), to be added
More than 3%, therefore, one layer of SEI film is previously generated on negative plate surface, battery initial charge capacitance loss can be reduced, so as to
Improve battery capacity.Meanwhile from table 1 it can also be seen that in embodiment 1-4, the electricity of lithium ion battery prepared by embodiment 3
Tankage is maximum, and the battery capacity of lithium ion battery prepared by embodiment 4 is minimum, and this also illustrates, the battery low current charge time
Longer, the generation of SEI films is more complete, and battery capacity is higher；Charging current is big, and SEI films generation effect is bad, influences battery capacity.
As shown in the above, the present invention forms one layer of SEI film by elder generation on negative plate, is then carried out again with positive plate
Be assembled into battery, avoid first formed in traditional approach battery again by preliminary filling formed SEI films so as to caused by reversible capacity damage
Lose, reduce the waste of material, saved the consumption of high-purity lithium, reduce battery cost；And reduce battery initial charge appearance
Amount loss, so as to improve battery capacity.The processing method of anode plate for lithium ionic cell of the present invention is implemented simple, it is easy to accomplish, it is complete
The industrialized production of lithium ion battery can be applied to scale entirely.
Those of ordinary skills in the art should understand that：The discussion of any of the above embodiment is exemplary only, not
It is intended to imply that the scope of the present disclosure (including claim) is limited to these examples；Under the thinking of the present invention, above example
Or can also be combined between the technical characteristic in different embodiments, and the different aspect of the present invention as described above be present
Many other changes, in order to it is concise they do not provided in details.Therefore, within the spirit and principles of the invention,
Any omission for being made, modification, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (7)
1. a kind of processing method of anode plate for lithium ionic cell, it is characterised in that anode plate for lithium ionic cell advances in winding
Row pretreatment, makes anode plate for lithium ionic cell surface previously generate one layer of SEI film.
2. the processing method of anode plate for lithium ionic cell according to claim 1, it is characterised in that bear lithium ion battery
Pole piece is put into electrolyte, enters line precharge, and charging current is 0.01~0.05C, and the charging interval is 2~6 hours, shelves 4~6
Minute, then anode plate for lithium ionic cell is discharged into 0.2V, placed 4~6 hours under vacuum, until anode plate for lithium ionic cell table
After face is dried.
3. the processing method of anode plate for lithium ionic cell according to claim 1, it is characterised in that the lithium ion battery
Negative plate is graphite cathode piece, and the electrolyte is lithium hexafluorophosphate electrolyte solution.
4. a kind of anode plate for lithium ionic cell, it is characterised in that according to the lithium ion battery described in any one of claims 1 to 3
The processing method of negative plate is prepared.
5. a kind of lithium ion battery, it is characterised in that including the anode plate for lithium ionic cell described in claim 4.
6. lithium ion battery according to claim 5, it is characterised in that also including casing of lithium ion battery, the lithium from
The pole piece for being previously generated the negative plate of one layer of SEI film and barrier film by positive plate, surface and being formed is provided with sub- battery case, lithium from
Injection electrolyte in sub- battery case, the electrolyte is lithium hexafluorophosphate electrolyte solution.
7. lithium ion battery according to claim 6, it is characterised in that the positive plate is lithium cobaltate cathode piece, described
Electrolyte is lithium hexafluorophosphate electrolyte solution, and the barrier film is cegard23 barrier films.
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Cited By (5)
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| CN109546226A (en) * | 2018-10-31 | 2019-03-29 | 湖南格兰博智能科技有限责任公司 | Negative electrode of lithium ion battery prelithiation method and lithium ion battery |
| CN111342028A (en) * | 2020-03-20 | 2020-06-26 | 金妍 | Formation method of lithium ion battery with graphite-based cathode |
| CN112635709A (en) * | 2020-12-15 | 2021-04-09 | 合肥工业大学 | SEI film forming agent for negative electrode of sodium-ion battery, pre-sodium treatment method and sodium-ion battery |
| CN113471428A (en) * | 2021-05-20 | 2021-10-01 | 福建海峡石墨烯产业技术研究院有限公司 | Method for improving graphite or graphene negative electrode stability of potassium ion battery and potassium ion battery |
| CN113793990A (en) * | 2021-09-15 | 2021-12-14 | 中国科学院长春应用化学研究所 | Method for improving rate capability of lithium ion battery by artificially synthesizing specific solid electrolyte interface film |
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| CN111342028A (en) * | 2020-03-20 | 2020-06-26 | 金妍 | Formation method of lithium ion battery with graphite-based cathode |
| CN112635709A (en) * | 2020-12-15 | 2021-04-09 | 合肥工业大学 | SEI film forming agent for negative electrode of sodium-ion battery, pre-sodium treatment method and sodium-ion battery |
| CN113471428A (en) * | 2021-05-20 | 2021-10-01 | 福建海峡石墨烯产业技术研究院有限公司 | Method for improving graphite or graphene negative electrode stability of potassium ion battery and potassium ion battery |
| CN113793990A (en) * | 2021-09-15 | 2021-12-14 | 中国科学院长春应用化学研究所 | Method for improving rate capability of lithium ion battery by artificially synthesizing specific solid electrolyte interface film |
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