CN113036149B - Dry-method positive electrode plate of lithium ion secondary battery and preparation method thereof - Google Patents
Dry-method positive electrode plate of lithium ion secondary battery and preparation method thereof Download PDFInfo
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- CN113036149B CN113036149B CN202110235288.0A CN202110235288A CN113036149B CN 113036149 B CN113036149 B CN 113036149B CN 202110235288 A CN202110235288 A CN 202110235288A CN 113036149 B CN113036149 B CN 113036149B
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/668—Composites of electroconductive material and synthetic resins
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0421—Methods of deposition of the material involving vapour deposition
- H01M4/0423—Physical vapour deposition
- H01M4/0426—Sputtering
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
The invention belongs to the technical field of preparation of positive pole pieces of lithium batteries, and particularly relates to a dry-method positive pole piece of a lithium ion secondary battery and a preparation method thereof. The positive electrode plate of the lithium ion secondary battery provided by the invention is of a sandwich structure, and the sequence is as follows: electrode coating, metal foil, electrode coating; the electrode coating includes: the positive electrode material comprises a carrier, a positive electrode main material and a conductive agent, wherein the positive electrode main material and the conductive agent are loaded in or on the surface of the carrier; the carrier is PTFE non-woven fabric. According to the invention, the composite mode of the positive pole piece is changed, so that the loading capacity of active substances in the pole piece and the dispersion uniformity of the active substances and PTFE in the pole piece are improved, the resistance of the pole piece is obviously reduced, and the electrical property of the pole piece is improved; meanwhile, no organic solvent is involved, no NMP waste gas is discharged, and the material cost of the battery is saved by 5-10%; because of no drying procedure, the manufacturing cost is saved by 40-60%.
Description
Technical Field
The invention belongs to the technical field of preparation of positive pole pieces of lithium batteries, and particularly relates to a dry-method positive pole piece of a lithium ion secondary battery and a preparation method thereof.
Background
The preparation flow of the positive electrode plate of the lithium ion secondary battery is as follows: batching, slurry mixing, coating, hot pressing and slitting; wherein the key steps are slurry mixing and coating procedures. At present, the slurry mixing is mainly finished by a wet preparation process, namely, the mixing of ingredients is realized by adding an organic solvent; for example, the most common slurry mixing process of the positive electrode sheet is: uniformly mixing an active substance, a conductive agent and a binder PVDF (polyvinylidene fluoride), gradually adding an organic solvent NMP (N-methylpyrrolidone) into the mixture, and preparing a slurry with a certain solid content. And extruding and spraying the obtained slurry on the surface of the metal current collector by a coating machine, drying, and entering the next working procedure.
However, the problems of the existing slurry mixing and coating procedures adopting the wet preparation process are mainly as follows:
(1) The use amount of the organic solvent NMP is large, the unit price is high, and the recovered NMP cannot be reused, so that the manufacturing cost of the battery is high;
(2) During the drying process, a part of organic solvent NMP is discharged in the form of waste gas, so that the environment is possibly polluted;
(3) After drying, a trace amount of organic solvent NMP remains in the positive electrode plate, and the battery performance is cracked;
(4) With the recovery of the organic solvent, the binder floats upwards in the drying process, so that the resistivity of the battery is increased, and the performance of the battery is reduced;
(5) The drying process accounts for 40-55% of the total energy consumption in the battery manufacturing process, so that the battery manufacturing cost is high.
In order to solve the problems of the wet preparation process, the prior art proposes to complete the mixing of electrode materials under the condition of no solvent, such as CN111725477A, the method grows graphene on the outer layer of the active particles by chemical vapor deposition or electrostatic spraying, and then the polymer binder is wrapped on the outer layers of the active particles and the graphene by electrostatic spraying to obtain the dry material which is uniformly mixed. However, the manufacturing cost of the dry material of the method is higher, and the preparation mode of forming the pole piece by compounding the dry material of the layer structure and the metal foil is not provided; because of the binder coating form adopted by the method, based on the current preparation technology of the positive electrode plate, the positive electrode plate with lower resistance is difficult to obtain by the skilled in the art.
Disclosure of Invention
The first aspect of the present invention provides a positive electrode sheet for a lithium ion secondary battery, which has a low resistance, and avoids a series of problems caused by the use of an organic solvent, such as environmental pollution, solvent residues, floating of a binder, large drying energy consumption, and the like, because no organic solvent is involved in the preparation of the raw materials.
The invention provides a positive electrode plate of a lithium ion secondary battery, which is of a sandwich structure and sequentially comprises the following components in sequence: electrode coating, metal foil, electrode coating;
the electrode coating includes: the positive electrode material comprises a carrier, a positive electrode main material and a conductive agent, wherein the positive electrode main material and the conductive agent are loaded in or on the surface of the carrier; the carrier is PTFE (polytetrafluoroethylene) non-woven fabric.
In the prior art, a conventional non-woven fabric is used as a carrier, and metal paste is coated on the inner part or the surface of the non-woven fabric in a sputtering mode, so that a metal layer is formed, and a current collector is obtained. The current collector has the advantages of lower resistance, lighter weight and the like, and can improve the charge and discharge performance of the lithium ion battery by loading active substances through the binder. However, the research of the invention finds that the current collector has less loading amount of active substances in the subsequent electrode pole piece preparation process due to the existence of the metal layer, and the active substances and the binder are unevenly dispersed in the carrier, so that the electrical performance of the obtained pole piece cannot reach the expectations.
Therefore, the invention provides a novel composite structure, namely, PTFE non-woven fabrics are used as carriers to load active substances such as positive electrode main materials, conductive agents and the like, so as to form an electrode coating; and then the electrode coating and the metal foil are compounded into an electrode plate in a sandwich structure. According to the invention, through changing the pole piece composite structure, the loading capacity of active substances in the pole piece and the dispersion degree of the active substances and PTFE in the pole piece are improved, so that the resistance of the pole piece is obviously reduced, and the electrical property of the pole piece is improved; meanwhile, the raw materials do not involve organic solvents, so that the problems in the wet preparation process are avoided.
The carrier of the invention has an areal density of 3-50g/m 2 The porosity is 10-90%. Specifically, the method can be determined according to the actual requirements of the positive pole piece. As one of the specific embodiments of the present invention, the areal density of the carrier is controlled to be 10-12g/m 2 The porosity is 70-80%, and the higher binding force between the carrier and the active substance and the higher loading capacity of the active substance are considered.
According to the invention, the research shows that although the improvement of the loading capacity of the powder is beneficial to the reduction of the resistance of the electrode, the uneven dispersion of the active substances in the carrier is easily caused by the excessive loading capacity, and the binding force between the active substances and the carrier is reduced, so that the electric performance of the pole piece is influenced. The invention thus controls the areal density of the electrode coating to 170-190g/m 2 。
The electrode coating is obtained by spraying powder containing a positive electrode main material and a conductive agent on the inside or the surface of a carrier through a sputtering technology. The loading capacity and the dispersion degree of the active substances in the carrier can be improved through the sputtering technology, and the combination capacity of the active substances and the carrier is improved, so that the resistance of the pole piece is obviously reduced.
The powder is prepared by kneading by high-speed dispersing equipment, and the linear speed of kneading can be determined according to the specific composition of the powder, and is usually between 5 and 100 m/s. Because the powder has no binder, the powder can be mixed more uniformly by adopting a kneading mode of a high-speed dispersing machine.
As one of the specific embodiments of the invention, the powder is obtained by mixing a positive electrode main material and a conductive agent through high-speed dispersing equipment; the linear speed of the mixing is controlled to be 25-60m/s. Research shows that the obtained powder can be more uniformly dispersed in the carrier or on the surface through sputtering by controlling the mixing speed, and meanwhile, the conductive agent powder particles are also beneficial to coating the surface of the positive electrode main material powder, so that the resistance of the pole piece is reduced.
Wherein the mass ratio of the positive electrode main material to the conductive agent is (90-99) to (1-10).
In order to obtain better loading effect, the invention also carries out intensive research on sputtering process conditions, including aspects of sputtering direction, sputtering distance, carrier temperature and the like.
In the preparation process of the electrode coating, the sputtering direction is vertical to the surface of the carrier, and the sputtering speed is 5-30m/s. Researches show that if the operation condition is unreasonably set, the powder is loaded in the carrier too little, and the electrode performance is affected; however, too much load can lead to uneven dispersion of active materials and also affect the performance of the electrode; therefore, the invention can ensure that the powder has a certain load capacity in the carrier and ensure that the powder is uniformly dispersed in the carrier by controlling the powder mixing condition and the sputtering speed, thereby obviously improving the electrode performance of the positive electrode plate.
In the preparation process of the electrode coating, the distance between the sputtering nozzle and the carrier can be determined according to actual requirements, and the distance range is between 10 and 200 mm.
As one of specific embodiments of the invention, the sputtering direction is vertical to the surface of the carrier, the sputtering speed is controlled to be 10-20m/s, and the distance between the sputtering nozzle and the carrier is 40-100mm. Under the condition, the loading and dispersion degree of the active material in the obtained electrode coating reach the optimal balance, and the resistance of the electrode plate is reduced more favorably.
In order to further improve the binding force of the powder and the carrier, the temperature of the carrier is controlled to be 110-120 ℃ before sputtering.
In order to further improve the loading capacity and the dispersion degree of the powder in the carrier, the carrier is in a negative pressure environment in the sputtering process, and the negative pressure interval is controlled to be-0.085 to 0MPa so as to prevent the powder from escaping and ensure that all the powder is loaded in or on the surface of the carrier as much as possible. In the implementation, the negative pressure device is arranged on the non-sputtering back surface of the carrier, and the negative pressure range is adjusted.
In the electrode coating, the positive electrode main material is one or more of lithium iron phosphate, ternary nickel cobalt manganese, ternary nickel cobalt aluminum, lithium cobaltate, lithium manganate or lithium iron manganese phosphate. The conductive agent is one or more of SP, carbon nano tube, carbon fiber, vgcf and the like.
The metal foil is aluminum foil. The thickness of the metal foil is 5-100 mu m.
The second aspect of the invention provides a preparation method of the positive electrode plate, comprising the steps of sequentially superposing an electrode coating, a metal foil and an electrode coating to obtain a large electrode plate; the superposition is realized by a hot pressing and electromagnetic induction heating procedure.
Research shows that PTFE can be uniformly dispersed in a large pole piece through hot pressing and electromagnetic induction heating processes, so that the bonding strength of an active substance and a carrier and the bonding strength between an electrode coating and a metal foil are improved, and the resistance of the pole piece is obviously reduced and the electrode performance is improved through multiple functions.
In the preparation method of the invention, the hot pressing conditions are as follows: the temperature is 80-220 ℃, preferably 170-220 ℃ and the time is 10-120s. The electromagnetic induction heating conditions are as follows: the power is 30-100KW, preferably 30-60KW, for 10-300s. The specific parameters are set according to the specific conditions of the actual coating and the metal foil.
As one of the specific embodiments of the present invention, the electrode coating has an areal density of 170-190g/m 2 The metal foil is aluminum foil, and the thickness of the metal foil is 10-20 mu m; conditions of the hot pressingThe method comprises the following steps: the temperature is 185-210 ℃ and the time is 25-45s; the electromagnetic induction heating conditions are as follows: the power is 30-60KW, and the time is 15-18s. By reasonably controlling the operation conditions, the dispersion uniformity of PTFE and the bonding force between layers are improved.
The preparation method also comprises the step of slitting the obtained large pole piece, and the specific slitting size is determined according to actual requirements.
The beneficial effects of the invention are as follows:
(1) The preparation process of the positive electrode plate does not involve organic solvent, no NMP waste gas is discharged, the environment is friendly, and the cost of battery materials is saved by 5-10%. Correspondingly, the preparation method also has no drying procedure, and the manufacturing cost is saved by 40-60%.
(2) The invention adopts a specific composite structure, so that no adhesive is needed in the batching process, the powder mixing degree is improved, and meanwhile, the loading capacity of active substances and the dispersion degree of the active substances in a carrier are improved, thereby obviously reducing the resistance of the pole piece.
(3) The invention makes PTFE uniformly distributed in the electrode through a specific superposition mode, and the cell resistance is 2-10% lower than that of the traditional method.
Detailed Description
The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
Each of the components in the examples below is commercially available.
Example 1
The embodiment provides a preparation method of a lithium iron phosphate positive electrode plate of a lithium ion secondary battery, which comprises the following steps:
(1) Powder material preparation: uniformly mixing the positive electrode main material powder and the conductive agent SP for 2 hours by a high-speed dispersing and kneading machine, wherein the linear speed is 25m/s, so as to obtain powder; the mass ratio of the positive electrode main material to the conductive agent in the obtained powder is 96:4;
(2) Preheating a carrier: 70% porosity, 10g/m 2 Heating the PTFE non-woven fabric with the surface density to 120 ℃, and placing the PTFE non-woven fabric at a position which is 40mm away from the right lower part of a high-speed sprayer;
(3) And (3) manufacturing an electrode coating: the mixed powder is arranged in a high-speed sprayerSpraying at 10m/s vertically downwards, sputtering inside and on the surface of PTFE non-woven fabric to obtain the surface density of 170g/m 2 Is a coating of an electrode; the lower part of the PTFE non-woven fabric is provided with a negative pressure device, and the negative pressure is minus 0.085MPa;
(4) Manufacturing a large pole piece: the electrode coating, the aluminum foil with the thickness of 15 mu m and the electrode coating are stacked in this order and hot-pressed, and the hot-pressing conditions are as follows: the temperature is 200 ℃, and the hot pressing time is 25 seconds; then passing through a 15m long battery induction heating area, wherein the electromagnetic induction heating power is 30KW, and the heating time is 15 seconds, so as to form a large pole piece; PTFE is uniformly dispersed in the large pole piece in the hot pressing process and the electroceramic induction heating process;
(5) And after the large pole piece is cut, forming the positive pole piece.
Example 2
The embodiment provides a preparation method of a ternary nickel cobalt lithium manganate positive plate of a lithium ion secondary battery, which comprises the following steps:
(1) Powder material preparation: uniformly mixing the positive electrode main material powder and the conductive agent SP for 2 hours by a high-speed dispersing and kneading machine, wherein the linear speed is 30m/s, so as to obtain powder; the mass ratio of the positive electrode main material to the conductive agent in the obtained powder is 97:3;
(2) Preheating a carrier: will have a porosity of 80% and a porosity of 10g/m 2 Heating the PTFE non-woven fabric with the surface density to 120 ℃, and placing the PTFE non-woven fabric at a position which is 60mm away from the lower part of a high-speed sprayer;
(3) And (3) manufacturing an electrode coating: the mixed powder is sprayed vertically downwards in a high-speed sprayer at a speed of 15m/s and is sputtered on the inner part and the surface of the PTFE non-woven fabric to form the powder with the surface density of 180g/m 2 Is a coating of an electrode; the PTFE lower part is provided with a negative pressure device, and the negative pressure is-0.085 MPa;
(4) Manufacturing a large pole piece: sequentially stacking and hot-pressing electrode coating, aluminum foil with thickness of 12 mu m and electrode coating, wherein the hot-pressing conditions are as follows: the temperature is 185 ℃, and the hot pressing time is 45 seconds; after hot pressing, passing through a 15m long battery induction heating area, wherein the electromagnetic induction heating power is 50KW, and the heating time is 15 seconds, so as to form a large pole piece; the adhesive is uniformly dispersed in the large pole piece in the hot pressing process and the electric porcelain induction heating process;
(5) And after the large pole piece is cut, forming the positive pole piece.
Example 3
The embodiment provides a preparation method of a lithium manganate positive electrode plate of a lithium ion secondary battery, which comprises the following steps:
(1) Powder material preparation: uniformly mixing the positive electrode main material powder and the conductive agent SP for 2 hours by a high-speed dispersing and kneading machine, wherein the linear speed is 30m/s, so as to obtain powder; the mass ratio of the positive electrode main material to the conductive agent in the obtained powder is 95:5;
(2) Preheating a carrier: will have a porosity of 80%, 12g/m 2 Heating the PTFE non-woven fabric with the surface density to 120 ℃, and placing the PTFE non-woven fabric at a position which is 100mm away from the right lower part of a high-speed sprayer;
(3) And (3) manufacturing an electrode coating: the mixed powder is sprayed vertically downwards in a high-speed sprayer at a speed of 20m/s and is sputtered on the inner part and the surface of the PTFE non-woven fabric to form the powder with the surface density of 190g/m 2 Is a coating of an electrode; the PTFE lower part is provided with a negative pressure device, and the negative pressure is-0.085 MPa;
(4) Manufacturing a large pole piece: sequentially stacking and hot-pressing electrode coating, aluminum foil with the thickness of 20 mu m and the electrode coating, wherein the hot-pressing conditions are as follows: the temperature is 210 ℃, and the hot pressing time is 40 seconds; after hot pressing, passing through a 15m long battery induction heating area, wherein the electromagnetic induction heating power is 60KW, and the heating time is 18 seconds, so as to form a large pole piece; the adhesive is uniformly dispersed in the large pole piece in the hot pressing process and the electric porcelain induction heating process;
(5) And after the large pole piece is cut, forming the positive pole piece.
Example 4
The present embodiment provides a preparation method of a lithium manganate positive electrode plate of a lithium ion secondary battery, which is different from embodiment 1 only in that: the surface density of the PTFE non-woven fabric is 30g/m 2 The porosity is 50%.
Example 5
The present embodiment provides a preparation method of a lithium manganate positive electrode plate of a lithium ion secondary battery, which is different from embodiment 1 only in that: the powder is prepared by mixing at a linear speed of 60m/s by a high-speed dispersing and kneading machine.
Example 6
The present embodiment provides a preparation method of a lithium manganate positive electrode plate of a lithium ion secondary battery, which is different from embodiment 1 only in that: and no negative pressure is set.
And (3) effect verification:
test example 1: the surface density of a single surface of a coating of the anode plate prepared by the traditional wet method is 170g/m 2 The mass fraction of PVDF binder in the pole piece is 5%.
The positive electrode sheets obtained in examples 1 to 6 and test example 1 were assembled into batteries, and the battery resistance was measured. The results were as follows:
TABLE 1
| Test example 1 | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Resistor | 20.8 | 19.4 | 18.8 | 19 | 19.7 | 19.3 | 20.2 |
| Reducing the amplitude of a beam | - | -6.73％ | -9.62％ | -8.65％ | -5.29％ | -7.21％ | -2.88％ |
Compared with test example 1, the battery resistances corresponding to the electrode plates obtained in examples 1 to 6 are reduced to a certain extent; the composite structure of the invention can obviously improve the electrical property of the pole piece. Whereas in example 6, the amplitude reduction is relatively small due to the absence of negative pressure means.
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (4)
1. The positive pole piece of the lithium ion secondary battery is characterized by being of a sandwich structure, and the sequence is as follows: electrode coating, metal foil, electrode coating;
the electrode coating includes: the positive electrode material comprises a carrier, a positive electrode main material and a conductive agent, wherein the positive electrode main material and the conductive agent are loaded in the carrier and on the surface of the carrier; the carrier is PTFE non-woven fabric;
the carrier has an areal density of 3-50g/m 2 Porosity is 10-90%; the surface density of the electrode coating is 170-190g/m 2 ；
The electrode coating is obtained by spraying powder containing a positive electrode main material and a conductive agent on the inside and the surface of a carrier through a sputtering technology;
the powder is obtained by mixing the positive electrode main material and the conductive agent through high-speed dispersing equipment; the linear speed of the mixing is controlled to be 25-60m/s;
the sputtering direction is vertical to the surface of the carrier, and the sputtering speed is 5-30m/s;
the distance between the sputtering nozzle and the carrier is 40-100mm;
before the sputtering, controlling the temperature of the carrier to be 110-120 ℃;
in the sputtering process, the carrier is in a negative pressure environment; the negative pressure interval is controlled to be-0.085 to 0Mpa.
2. The positive electrode tab of a lithium ion secondary battery according to claim 1, wherein the carrier has an areal density of 10 to 12g/m 2 The porosity is 70-80%.
3. The method for preparing the positive electrode sheet of the lithium ion secondary battery as claimed in claim 1 or 2, which is characterized by comprising the step of sequentially superposing an electrode coating, a metal foil and an electrode coating to obtain a large electrode sheet; the superposition is realized by a hot pressing and electromagnetic induction heating procedure.
4. The method for preparing a positive electrode sheet of a lithium ion secondary battery according to claim 3, wherein the surface density of the electrode coating layer is 170-190g/m 2 The metal foil is aluminum foil, and the thickness of the metal foil is 10-20 mu m; the hot pressing conditions are as follows: the temperature is 185-210 ℃ and the time is 25-45s; the electromagnetic induction heating conditions are as follows: the power is 30-60KW, and the time is 15-18s.
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