CN113964293B - Cyclic stable quick-charging type lithium ion battery cathode and application thereof - Google Patents
Cyclic stable quick-charging type lithium ion battery cathode and application thereof Download PDFInfo
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- CN113964293B CN113964293B CN202111114207.8A CN202111114207A CN113964293B CN 113964293 B CN113964293 B CN 113964293B CN 202111114207 A CN202111114207 A CN 202111114207A CN 113964293 B CN113964293 B CN 113964293B
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a negative electrode of a circularly stable and fast-charging lithium ion battery and application thereof. According to the invention, the three layers of cathode slurry coatings with the gradient distribution of the specific surface area of the conductive additive are added into the cathode of the lithium ion battery, and the conductive additive is distributed according to the time constant ratio to form a hierarchical electrode structure, so that the distribution rule of the longitudinal potential gradient and the ion concentration gradient of the electrode is met, and the uniformity of the longitudinal dynamic reaction rate of the electrode can be improved; meanwhile, an electric double layer mechanism which responds preferentially under large current is introduced to be used as a buffer, so that the negative electrode is charged uniformly in a reverse direction, and the uniformity of local reaction kinetics can be improved. Under the synergistic effect of the two functions, the lithium precipitation and mechanical damage of the negative electrode under the condition of large-current cycle are inhibited, and the high-rate and long-cycle stability are achieved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a cathode of a circularly stable and fast-charging lithium ion battery and application thereof.
Background
At present, the key to limit the popularization of electric vehicles lies in the performance lag of power devices (lithium ion batteries) and causes users to face greater mileage anxiety. To solve this problem, two possible technical routes are: 1. the energy density of the lithium ion battery is improved, and the single charging endurance mileage of the electric automobile is increased; 2. the multiplying power performance of the lithium ion battery is improved, and the charging time of the electric automobile is shortened. Among them, the former is the main research direction in recent years, and the measure is to use a high-voltage and high-specific-capacity NCM or NCA positive electrode instead of the conventional LFP positive electrode. However, the above materials suffer from poor thermal/structural stability, oxygen evolution and manganese dissolution during cycling, which poses a significant safety hazard for high specific energy devices. Therefore, more and more research institutes focus on fast-charging lithium ion batteries.
The problems of the fast-charge lithium ion battery are mainly concentrated on the negative electrode side. The negative electrode material of a lithium ion battery is generally graphite, soft carbon, hard carbon, and the like, which undergoes an intercalation reaction with lithium ions during charge and discharge. Since the reaction involves diffusion mass transfer of lithium ions in the solid phase of the electrode material and has poor reaction kinetics, a great deal of research and development work is focused on the structural design of the material to improve the solid phase diffusion coefficient of the lithium ions, thereby increasing the rate capability. However, a key problem that has not yet been solved is that, in an actual cycling process, due to differences of local structures of electrode materials and electrodes, and uneven distribution of current density and ion concentration in the electrodes, mismatch phenomena of local reaction polarization and reaction strain (including mismatch on a macroscopic longitudinal scale of the electrodes and microscopic local mismatch caused by various anisotropies of active materials) are caused, and particularly under the conditions of thicker electrodes and larger charging currents, problems such as lithium precipitation, SEI growth, structural damage of the electrodes and the like are caused, so that cycling stability of the electrodes is reduced, and potential safety hazards are caused.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a circularly stable and fast-charging lithium ion battery cathode which has uniform current density and ion concentration distribution, and reduces the risk of lithium precipitation caused by local excessive polarization and the damage of an electrode structure caused by strain mismatch.
The purpose of the invention can be realized by the following technical scheme:
the utility model provides a circulation is stable fills type lithium ion battery negative pole soon, includes mass flow body and negative pole slurry coating, and negative pole slurry coating from the bottom up includes bottom, intermediate level, top layer in proper order, and wherein the bottom coating is on the mass flow body surface, and bottom, intermediate level, top layer all include conductive additive B, and conductive additive B's specific surface area reduces from bottom to top layer direction gradient.
Preferably, the total thickness of the negative electrode slurry coating is 90 to 120 μm.
Preferably, the surface loading of the negative electrode slurry coating on the surface of the current collector is 8-15mg/cm 2 。
In the cathode of the cycling stable quick-charging type lithium ion battery, the cathode slurry comprises the following raw materials in parts by mass: 90-95 parts of active substance, 1.25-2.5 parts of conductive additive A, 1.25-2.5 parts of conductive additive B and 2.5-5 parts of binder.
Preferably, the active material is one or more of graphite, soft carbon, and hard carbon.
Preferably, the binder is one or more of styrene butadiene rubber, carboxymethyl cellulose, polytetrafluoroethylene and polyvinylidene fluoride.
In the negative electrode of the cycling stable quick-charging type lithium ion battery, the specific surface area of the conductive additive B in the bottom layer is 800-1500m 2 (ii)/g, the specific surface area of the conductive additive B in the intermediate layer is 400 to 700m 2 (ii)/g, the specific surface area of the conductive additive B in the top layer is from 200 to 300m 2 /g。
In the negative electrode of the cycling stable quick-charging type lithium ion battery, the conductive additive A is carbon black.
In the negative electrode of the cycling stable quick-charging type lithium ion battery, the conductive additive B is one or more of Ketjen black, single-walled carbon nanotube and graphene.
In the negative electrode of the fast-charging lithium ion battery with stable cycle, the time constant (tau = RC) ratio of the conductive additive B in the bottom layer, the middle layer and the top layer is (3-5): (1.5-2): (0.8-1). The time constant reflects the rate of electric double layer response of conductive additive B, i.e., the time required to complete charging.
According to the invention, through the electrode structure design with gradient distribution of the specific surface and the customized time constant proportion control, the ion concentration and the potential distribution on the longitudinal scale of the electrode are changed, and the dynamic uniformity of the lithium intercalation reaction on the longitudinal scale of the electrode is promoted, so that the risk of lithium precipitation and structure damage caused by overhigh local overpotential of the electrode under the rapid charging condition is reduced. In addition, the conductive additive with high specific surface area can also be used as a charging buffer of the lithium intercalation reaction by introducing an electric double layer energy storage mechanism with quick response characteristic, namely, the conductive additive is preferentially responded in the charging process and then carries out charge transmission on the lithium intercalation reaction material, so that the current density of the lithium intercalation reaction is reduced, and the kinetic uniformity of the microscopic local reaction of the lithium intercalation material is further improved.
The invention also provides a button cell which comprises the cathode of the cycling stable quick-charging type lithium ion battery.
The invention also provides a preparation method of the button cell, which comprises the following steps:
s1, preparing slurry of the bottom layer, the middle layer and the top layer;
s2, sequentially coating the slurry of the bottom layer and the slurry of the middle layer on a copper foil current collector in a scraping manner, and respectively drying;
s3, coating the top layer slurry on the middle layer slurry in a scraping mode, and then carrying out drying treatment;
s4, pressing into a negative pole piece;
s5, assembling the negative pole piece, the diaphragm and the lithium piece into a button cell in a sandwich structure;
and S6, carrying out chemical treatment on the button cell by adopting constant current pulse.
The invention realizes the low current charging of the active material by utilizing the preferential response of the conductive additive based on the quick dynamic response double electric layer reaction mechanism in the pulse process and the charge redistribution effect in the relaxation process, thereby improving the dynamic uniformity of the SEI film forming reaction and obtaining the high-quality SEI film.
Preferably, the thickness of the negative pole piece is 1-2cm.
Preferably, the electrolyte of the button cell is conventional LiPF 6 /EC/EMC/DMC。
Preferably, the drying treatment temperature of the step S2 is 95-120 ℃, and the drying treatment time is 2-3h.
Preferably, the drying treatment temperature of the step S3 is 95-105 ℃ and the time is 5-8h.
Preferably, the formation treatment specifically comprises: and charging the potential of the cathode of the button cell to 0.8-1.2V by adopting a current value of 0.1-0.5C, then continuously charging for 10-30min by adopting a current value of 0.1-0.2C, standing for 10-20min, and circulating until the potential of the cathode is 0.005-0.01V.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the three-layer negative electrode slurry coating with the gradient distribution of the specific surface area of the conductive additive is added into the negative electrode of the lithium ion battery, and the conductive additive is distributed according to the time constant ratio to form a hierarchical electrode structure, so that the distribution rule of the longitudinal potential gradient and the ion concentration gradient of the electrode is met, and the uniformity of the longitudinal dynamic reaction rate of the electrode can be improved; meanwhile, an electric double layer mechanism which responds preferentially under large current is introduced to be used as a buffer, so that the negative electrode is charged uniformly in a reverse direction, and the uniformity of local reaction kinetics can be improved. Under the synergistic effect of the two functions, the lithium precipitation and mechanical damage of the negative electrode under the condition of large-current cycle are inhibited, and the high-rate and long-cycle stability are achieved.
Drawings
Fig. 1 is an 8C charge curve of a conventional lithium ion negative electrode.
Fig. 2 is an 8C charge curve of the fast-charging type negative electrode of example 1.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
Example 1:
s1, preparing slurry I, slurry II and slurry III from 94 parts of soft carbon, 1.5 parts of carbon black, 1.5 parts of Ketjen black and 3 parts of polyvinylidene fluoride in parts by mass; wherein the specific surface area of the paste I Ketjen black is 1023m 2 (ii) the specific surface area of the paste IIKetjen black is 412m 2 (iii) g, specific surface area of the paste IIIKetjen black is 231m 2 And the ratio of time constants (τ = RC) of paste i ketjen black, paste ii ketjen black, and paste iii ketjen black is 4.
S2、Sequentially carrying out blade coating on the slurry I, the slurry II and the slurry III on a copper foil current collector according to a thickness ratio of 1.2 2 。
And S3, compacting the dried negative electrode by using a roll machine, and punching the negative electrode into a negative electrode plate with the diameter of 1.2cm by using a punching machine.
S4, assembling the negative pole piece, the diaphragm and the lithium piece into a button cell in a sandwich structure, and adopting conventional lithium ion electrolyte (LiPF) 6 /EC/EMC/DMC)；
S5, carrying out formation treatment on the button cell: the button cell negative electrode potential was charged to 1.2V with 0.5C (1c = 372ma/g), followed by 20min with 0.2C and 10min at rest, cycling until the negative electrode potential was 0.01V.
Example 2:
the difference from example 1 is only that the ratio of time constants (τ = RC) of paste i ketjen black, paste ii ketjen black, and paste iii ketjen black is 1.
Example 3:
the difference from the example 1 is only that slurry I, slurry II and slurry III are sequentially coated on a copper foil current collector according to the thickness ratio of 1.5.
Example 4:
the only difference from example 1 is that the negative electrode was charged using a conventional chemical conversion treatment, i.e., at a current density of 0.1C.
Comparative example 1:
the difference from example 1 was only that the specific surface area of Ketjen black of slurry I and that of Ketjen black of slurry II were 412m 2 /g。
Comparative example 2:
the difference from example 1 was only that the specific surface area of Ketjen black of slurry I and that of Ketjen black of slurry III were 1023m 2 /g。
Comparative example 3:
the difference from the embodiment 1 is only that the slurry I and the slurry II are sequentially coated on the copper foil current collector by scraping, and the slurry III is not added.
Comparative example 4:
the difference from the example 1 is only that the slurry II and the slurry III are sequentially coated on the copper foil current collector by scraping, and the slurry I is not added.
Comparative example 5:
the difference from example 1 is that slurry i was knife coated on the copper foil current collector without adding slurry ii and slurry iii.
Table 1: test results of performance of button cell batteries of examples 1-4 and comparative examples 1-5
| Examples | Multiplying power performance (0.1C/8C) | Cycle performance (100 rings) |
| Example 1 | 38.7％ | 93.2％ |
| Example 2 | 22％ | 80％ |
| Example 3 | 32.6％ | 85.4％ |
| Example 4 | 33.5％ | 78.7％ |
| Comparative example 1 | 27％ | 87.3％ |
| Comparative example 2 | 23.2％ | 74％ |
| Comparative example 3 | 35.1％ | 85％ |
| Comparative example 4 | 32.8％ | 86.3％ |
| Comparative example 5 | 29％ | 76％ |
Fig. 1 is an 8C charge curve for a conventional lithium ion negative electrode; fig. 2 is an 8C charge curve of the fast-charging type negative electrode of example 1. It can be seen that under the high-rate charging condition, when the voltage curve of the conventional lithium ion battery negative electrode approaches the cut-off voltage (0.01V), a significant lithium deposition plateau occurs, while the fast-charging negative electrode of the present invention does not have a lithium deposition plateau.
In conclusion, the three-layer negative electrode slurry coating with the conducting additive distributed in the specific surface area in a gradient manner is added into the negative electrode of the lithium ion battery, and the conducting additive is distributed according to the time constant ratio, so that a hierarchical electrode structure is formed, the distribution rules of the longitudinal electric potential gradient and the ion concentration gradient of the electrode are met, and the uniformity of the longitudinal kinetic reaction rate of the electrode can be improved; meanwhile, an electric double layer mechanism which responds preferentially under large current is introduced to serve as a buffer, so that the negative electrode is charged uniformly in a reverse direction, and the uniformity of local reaction kinetics can be improved. Under the synergistic effect of the two functions, the lithium precipitation and mechanical damage of the negative electrode under the condition of large-current cycle are inhibited, and the high-rate and long-cycle stability are achieved. In addition, as example 2 changes the coating sequence of the negative electrode, example 3 and comparative example 1 reduce the time constant ratio of the conductive additives in different levels, and comparative example 2 changes the distribution rule, example 4 adopts a conventional formation process, and comparative examples 4-6 reduce the coating layer number of the negative electrode slurry, which reduces the rate performance and the cycling stability.
The technical range of the embodiment of the invention is not exhaustive, and new technical solutions formed by equivalent replacement of single or multiple technical features in the technical solutions of the embodiment are also within the scope of the invention; in all the embodiments of the present invention, which are listed or not listed, each parameter in the same embodiment only represents an example (i.e., a feasible embodiment) of the technical solution, and there is no strict matching and limiting relationship between the parameters, wherein the parameters may be replaced with each other without departing from the axiom and the requirements of the present invention, unless otherwise specified.
The technical means disclosed by the scheme of the invention are not limited to the technical means disclosed by the technical means, and the technical means also comprises the technical scheme formed by any combination of the technical features. While the foregoing is directed to embodiments of the present invention, it will be appreciated by those skilled in the art that various changes may be made in the embodiments without departing from the principles of the invention, and that such changes and modifications are intended to be included within the scope of the invention.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. The utility model provides a circulation is stable fills type lithium ion battery negative pole soon, includes mass flow body and negative pole thick liquids coating, its characterized in that, negative pole thick liquids coating from the bottom up includes bottom, intermediate level, top layer in proper order, and wherein the bottom coating is on the mass flow body surface, and bottom, intermediate level, top layer all include conductive additive B, and conductive additive B's specific surface area reduces from bottom to top layer direction gradient.
2. The negative electrode of claim 1, wherein the specific surface area of the conductive additive B in the bottom layer is 800-1500m 2 (ii)/g, the specific surface area of the conductive additive B in the intermediate layer is 400 to 700m 2 (ii)/g, the specific surface area of the conductive additive B in the top layer is from 200 to 300m 2 /g。
3. The negative electrode of the cycling stable quick-charging type lithium ion battery as claimed in claim 1 or 2, wherein the negative electrode slurry comprises the following raw materials in parts by mass: 90-95 parts of active substance, 1.25-2.5 parts of conductive additive A, 1.25-2.5 parts of conductive additive B and 2.5-5 parts of binder.
4. The negative electrode of the cycling-stable fast-charging lithium ion battery of claim 3, wherein the conductive additive A is carbon black.
5. The negative electrode of the cycling stable fast-charging type lithium ion battery according to claim 3, wherein the conductive additive B is one or more of Ketjen black, single-walled carbon nanotube and graphene.
6. The negative electrode of a cycle-stable fast-charge lithium ion battery as claimed in claim 1 or 2, wherein the time constant (τ = RC) ratio of the conductive additive B in the bottom layer, the intermediate layer, and the top layer is (3-5): (1.5-2): (0.8-1).
7. The negative electrode of the lithium ion battery as claimed in claim 1 or 2, wherein the coating thickness ratio of the bottom layer, the middle layer and the top layer is 1 (1.1-1.3) to 1.4-1.6.
8. A button cell comprising the negative electrode of the cycling-stable, fast-charging lithium ion battery of claim 1.
9. A method for preparing a button cell according to claim 8, which comprises the following steps:
s1, preparing sizing agents of the bottom layer, the middle layer and the top layer;
s2, sequentially coating the slurry of the bottom layer and the slurry of the middle layer on a copper foil current collector in a scraping manner, and respectively drying;
s3, coating the top layer slurry on the middle layer slurry in a scraping mode, and then carrying out drying treatment;
s4, pressing into a negative pole piece;
s5, assembling the negative pole piece, the diaphragm and the lithium piece into a button cell in a sandwich structure;
and S6, carrying out chemical treatment on the button cell by adopting constant current pulse.
10. The button cell preparation method according to claim 9, wherein the formation treatment specifically comprises: and charging the potential of the negative electrode of the button cell to 0.8-1.2V by adopting a current value of 0.1-0.5C, then continuously charging for 10-30min by adopting a current value of 0.1-0.2C, standing for 10-20min, and circulating until the potential of the negative electrode is 0.005-0.01V.
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