CN113036149A - Dry-process positive pole piece of lithium ion secondary battery and preparation method thereof - Google Patents
Dry-process positive pole piece of lithium ion secondary battery and preparation method thereof Download PDFInfo
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- CN113036149A CN113036149A CN202110235288.0A CN202110235288A CN113036149A CN 113036149 A CN113036149 A CN 113036149A CN 202110235288 A CN202110235288 A CN 202110235288A CN 113036149 A CN113036149 A CN 113036149A
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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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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention belongs to the technical field of preparation of a lithium battery positive pole piece, and particularly relates to a dry-process positive pole piece of a lithium ion secondary battery and a preparation method thereof. The positive pole piece 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: a carrier, and a positive electrode main material and a conductive agent loaded in or on the surface of the carrier; the carrier is PTFE non-woven fabric. According to the invention, by changing the compound mode of the positive pole piece, the loading capacity of the active substance in the pole piece and the dispersion uniformity of the active substance 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, because no organic solvent is involved, NMP waste gas is not discharged, and the cost of the battery material is saved by 5-10%; because no drying procedure is carried out, the manufacturing cost is saved by 40-60%.
Description
Technical Field
The invention belongs to the technical field of preparation of a lithium battery positive pole piece, and particularly relates to a dry-process positive pole piece of a lithium ion secondary battery and a preparation method thereof.
Background
The preparation process of the positive pole piece of the lithium ion secondary battery comprises the following steps: batching → slurry mixing → coating → hot pressing → cutting; wherein the key steps are slurry mixing and coating procedures. The existing slurry mixing is mainly completed through a wet preparation process, namely, the mixture is mixed by adding an organic solvent; for example, the most commonly used slurry mixing process of the positive electrode plate is as follows: the active substance, the conductive agent and the PVDF (polyvinylidene fluoride) binder are uniformly mixed, and an organic solvent NMP (N-methyl pyrrolidone) is gradually added into the mixture to prepare slurry with 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 existing slurry mixing and coating processes adopting the wet preparation process mainly have the following problems:
(1) the organic solvent NMP has large dosage and high unit price, and the recovered NMP can not be reused, so that the manufacturing cost of the battery is high;
(2) in the drying process, a part of organic solvent NMP is discharged in the form of waste gas, so that the possibility of environmental pollution is high;
(3) after drying, a trace amount of organic solvent NMP remains in the positive pole piece, 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, resulting in higher manufacturing cost of the battery.
In order to solve the problems of the wet preparation process, the prior art proposes that the electrode material is mixed without the aid of a solvent, such as CN111725477A, in the method, graphene grows on the outer layer of the active particles by means of chemical vapor deposition or electrostatic spraying, and then a polymer binder is coated on the outer layer of the active particles and the graphene by means of electrostatic spraying, so as to obtain a uniformly mixed dry material. However, the manufacturing cost of the dry material of the method is high, and a preparation method for forming the pole piece by compounding the dry material of the layer structure and the metal foil is not provided; because the binder coating form adopted by the method is based on the preparation technology of the prior positive pole piece, the positive pole piece with lower resistance is difficult to obtain by the technical personnel in the field.
Disclosure of Invention
The first aspect of the invention provides a positive pole piece of a lithium ion secondary battery, which has lower resistance, and because the preparation raw materials do not relate to an organic solvent, a series of problems caused by the use of the organic solvent, such as environmental pollution, solvent residue, floating of a binder, high drying energy consumption and the like, are avoided.
The invention provides a positive pole piece of a lithium ion secondary battery, which is of a sandwich structure and sequentially comprises the following steps: electrode coating, metal foil, electrode coating;
the electrode coating includes: a carrier, and a positive electrode main material and a conductive agent 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 slurry is coated inside or on the surface of the non-woven fabric in a sputtering manner to form a metal layer, so that a current collector is obtained. The current collector has the advantages of low 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 existence of the metal layer causes the current collector to have less loading capacity on the active substance in the subsequent electrode pole piece preparation process, and the active substance and the binder are not uniformly dispersed in the carrier, so that the electrical property of the obtained pole piece cannot reach the expectation.
Therefore, the invention provides a novel composite structure, namely, PTFE non-woven fabric is taken as a carrier, active substances such as a positive electrode main material, a conductive agent and the like are loaded, and an electrode coating is formed; and compounding the electrode coating and the metal foil in a sandwich structure to form the electrode plate. According to the invention, by changing the composite structure of the pole piece, the loading capacity of the active substance in the pole piece and the dispersion degree of the active substance 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 relate to organic solvents, so that the problems in the wet preparation process are avoided.
The surface density of the carrier of the invention is 3-50g/m2And the porosity is 10-90%. The specific requirement can be determined according to the actual requirement of the positive pole piece. As one embodiment of the present invention, the areal density of the support is controlled to 10 to 12g/m2Porosity of 70-80%, andthe higher binding power between the carrier and the active material, and the higher loading of the active material, are taken into account.
The research of the invention finds that although the improvement of the loading capacity of the powder is beneficial to reducing the resistance of the electrode, the over-high loading capacity easily causes the uneven dispersion of the active substance in the carrier, and reduces the binding force between the active substance and the carrier, but influences the electrical property of the pole piece. Therefore, the invention controls the surface density of the electrode coating to be 170-190g/m2。
The electrode coating is obtained by spraying powder containing a positive electrode main material and a conductive agent into or on the surface of a carrier by 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 meanwhile, the binding capacity of the active substances and the carrier is improved, so that the resistance of the pole piece is obviously reduced.
The powder of the invention is prepared by kneading through a high-speed dispersion device, and the linear velocity of the kneading can be determined according to the concrete composition of the powder and is usually between 5 and 100 m/s. Because the powder is not provided with the adhesive, the powder can be mixed more uniformly by adopting a high-speed dispersion machine kneading mode.
In one embodiment of the present invention, the powder is obtained by kneading a positive electrode main material and a conductive agent by a high-speed dispersion apparatus; the linear speed of the mashup is controlled to be 25-60 m/s. Research shows that by controlling the mixing speed, the obtained powder can be more uniformly dispersed in the carrier or on the surface of the carrier through sputtering, and meanwhile, the conductive agent powder particles are also favorably coated on the surface of the positive electrode main material powder, so that the resistance of a 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 deep research on the sputtering process conditions, including the aspects of sputtering direction, sputtering distance, carrier temperature and the like.
In the preparation process of the electrode coating, the sputtering direction is required to be vertical to the surface of the carrier, and the sputtering speed is 5-30 m/s. Research shows that if the operation conditions are set unreasonably, the loading capacity of the powder in the carrier is too small, and the electrode performance is influenced; however, too much loading can lead to uneven dispersion of the active material and also affect the performance of the electrode; therefore, the invention can ensure that the powder has certain loading capacity in the carrier and 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 pole piece.
During 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 10-200 mm.
As one embodiment 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 40-100 mm. Under the condition, the loading capacity and the dispersion degree of the active substances in the obtained electrode coating reach the optimal balance, and the resistance of the pole piece is more favorably reduced.
In order to further improve the bonding force between the powder and the carrier, the temperature of the carrier is controlled to be 110-120 ℃ before the sputtering.
In order to further improve the loading amount and the dispersion degree of the powder in the carrier, in the sputtering process, the carrier is in a negative pressure environment, the negative pressure interval is controlled to be-0.085 to 0MPa, so that the powder is prevented from escaping, and all the powder is ensured to be loaded in the carrier or on the surface of the carrier as far as possible. In specific implementation, a 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 main material of the positive electrode 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 an aluminum foil. The thickness of the metal foil is 5-100 μm.
The second aspect of the invention provides a preparation method of the positive pole piece, which comprises the steps of superposing an electrode coating, a metal foil and the electrode coating in sequence to obtain a large pole piece; the lamination is realized by hot pressing and electromagnetic induction heating processes.
Researches show that PTFE can be uniformly dispersed in a large pole piece through hot pressing and electromagnetic induction heating processes, the bonding strength between an active substance and a carrier and the bonding strength between an electrode coating and a metal foil are improved, the resistance of the pole piece is obviously reduced through multiple actions, and the electrode performance is improved.
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 10-120 s. The electromagnetic induction heating conditions are as follows: the power is 30-100KW, preferably 30-60KW, and the time is 10-300 s. The specific parameters are set according to the specific conditions of the actual coating and the metal foil.
As one embodiment of the invention, the surface density of the electrode coating is 170-190g/m2The metal foil is an 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 25-45 s; the electromagnetic induction heating conditions are as follows: the power is 30-60KW, and the time is 15-18 s. By reasonably controlling the operating conditions, the dispersion uniformity of the PTFE and the bonding force among 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 the actual requirement.
The invention has the following beneficial effects:
(1) the preparation process of the positive pole piece does not involve an organic solvent, does not discharge NMP waste gas, is environment-friendly, and saves 5-10% of the material cost of the battery. Correspondingly, the preparation method 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 used in the material preparation process, the powder mixing degree is improved, and the loading capacity of the active substance and the dispersion degree of the active substance in the carrier are improved, thereby obviously reducing the resistance of the pole piece.
(3) The invention makes PTFE uniformly distributed in the electrode by a specific overlapping mode, and the battery resistance is 2-10% lower than that of the traditional method.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Each of the components in the following examples is commercially available.
Example 1
The embodiment provides a preparation method of a lithium iron phosphate positive pole piece of a lithium ion secondary battery, which comprises the following steps:
(1) powder proportioning: uniformly mixing the main anode material powder and the conductive agent SP for 2 hours by a high-speed dispersion kneading machine at a linear speed of 25m/s 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: the porosity of 70 percent and the density of 10g/m2Heating the PTFE non-woven fabric with the surface density to 120 ℃, and placing the PTFE non-woven fabric at a position with a distance of 40mm under a high-speed jet machine;
(3) preparing an electrode coating: the mixed powder was vertically sprayed downward at a speed of 10m/s in a high-speed sprayer, and sputtered into the inside and the surface of a PTFE nonwoven fabric to obtain an areal density of 170g/m2The electrode coating of (1); the lower part of the PTFE non-woven fabric is provided with a negative pressure device, and the negative pressure is-0.085 MPa;
(4) manufacturing a large pole piece: and stacking the electrode coating, the 15-micron thick aluminum foil and the electrode coating in this order, and hot-pressing under the conditions that: the temperature is 200 ℃, and the hot pressing time is 25 seconds; then passing through a 15m long battery induction heating zone, and heating by electromagnetic induction with the power of 30KW for 15 seconds to form a large pole piece; PTFE can be uniformly dispersed in the large pole piece in the hot pressing process and the electroceramic induction heating process;
(5) and cutting the large pole piece to form the positive pole piece.
Example 2
The embodiment provides a preparation method of a ternary nickel cobalt lithium manganate positive pole piece of a lithium ion secondary battery, which comprises the following steps:
(1) powder proportioning: uniformly mixing the main anode material powder and the conductive agent SP for 2 hours by a high-speed dispersion kneading machine at a linear speed of 30m/s 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: the porosity of 80 percent and the density of 10g/m2The PTFE non-woven fabric of areal density was heated to 120 c,placing the high-speed jet machine at a position with a distance of 60mm under the high-speed jet machine;
(3) preparing an electrode coating: the mixed powder is vertically sprayed downwards at a speed of 15m/s in a high-speed sprayer and is sputtered into the inner part and the surface of the PTFE non-woven fabric to form the surface density of 180g/m2The electrode coating of (1); the lower part of the PTFE is provided with a negative pressure device, and the negative pressure is between-0.085 MPa;
(4) manufacturing a large pole piece: and sequentially stacking the electrode coating, the 12-micron thick aluminum foil and the electrode coating and hot-pressing, 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 zone, heating by electromagnetic induction with the power of 50KW for 15 seconds to form a large pole piece; the adhesive is uniformly dispersed in the large pole piece in the hot pressing process and the electroceramic induction heating process;
(5) and cutting the large pole piece to form the positive pole piece.
Example 3
The embodiment provides a preparation method of a lithium manganate positive pole piece of a lithium ion secondary battery, which comprises the following steps:
(1) powder proportioning: uniformly mixing the main anode material powder and the conductive agent SP for 2 hours by a high-speed dispersion kneading machine at a linear speed of 30m/s 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: the porosity of 80 percent, 12g/m2Heating the PTFE non-woven fabric with the surface density to 120 ℃, and placing the PTFE non-woven fabric at a position with a distance of 100mm under a high-speed jet machine;
(3) preparing an electrode coating: the mixed powder was vertically sprayed downward at a speed of 20m/s in a high-speed sprayer, and sputtered into the inside and the surface of a PTFE nonwoven fabric to form a sheet having an areal density of 190g/m2The electrode coating of (1); the lower part of the PTFE is provided with a negative pressure device, and the negative pressure is between-0.085 MPa;
(4) manufacturing a large pole piece: and sequentially stacking the electrode coating, the aluminum foil with the thickness of 20 mu m and the electrode coating and hot-pressing, 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 zone, heating by electromagnetic induction with the power of 60KW for 18 seconds to form a large pole piece; the adhesive is uniformly dispersed in the large pole piece in the hot pressing process and the electroceramic induction heating process;
(5) and cutting the large pole piece to form the positive pole piece.
Example 4
The embodiment provides a preparation method of a lithium manganate positive electrode piece of a lithium ion secondary battery, which is different from the embodiment 1 only in that: the surface density of the PTFE non-woven fabric is 30g/m2And the porosity is 50%.
Example 5
The embodiment provides a preparation method of a lithium manganate positive electrode piece of a lithium ion secondary battery, which is different from the embodiment 1 only in that: the powder is prepared by mixing through a high-speed dispersion kneading machine at a linear speed of 60 m/s.
Example 6
The embodiment provides a preparation method of a lithium manganate positive electrode piece of a lithium ion secondary battery, which is different from the embodiment 1 only in that: no negative pressure is set.
Effect verification:
test example 1: the surface density of the single surface of the coating of the anode pole piece prepared by the traditional wet method is 170g/m2And the mass fraction of the PVDF binder in the pole piece is 5%.
The positive pole pieces obtained in examples 1 to 6 of the present application and test example 1 were assembled into a battery, and the battery resistance was tested. The results are as follows:
TABLE 1
| Test example 1 | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Resistance (RC) | 20.8 | 19.4 | 18.8 | 19 | 19.7 | 19.3 | 20.2 |
| Amplitude reduction | - | -6.73％ | -9.62％ | -8.65％ | -5.29％ | -7.21％ | -2.88％ |
As can be seen by comparison, the battery resistances corresponding to the electrode sheets obtained in examples 1 to 6 were all reduced to some extent as compared with test example 1; the composite structure of the invention can obviously improve the electrical property of the pole piece. And in the embodiment 6, the amplitude reduction is relatively small due to the non-negative pressure device.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The utility model provides a lithium ion secondary battery's positive pole piece which characterized in that, positive pole piece is sandwich structure, and the order is in proper order: electrode coating, metal foil, electrode coating;
the electrode coating includes: a carrier, and a positive electrode main material and a conductive agent loaded in or on the surface of the carrier; the carrier is PTFE non-woven fabric.
2. The positive electrode sheet for a lithium ion secondary battery according to claim 1, wherein the support has an areal density of 3 to 50g/m2The porosity is 10-90%;
preferably, the support has an areal density of 10 to 12g/m2The porosity is 70-80%.
3. The positive electrode plate of the lithium-ion secondary battery as claimed in claim 2, wherein the surface density of the electrode coating is 190g/m and 170-2。
4. The positive electrode sheet for a lithium-ion secondary battery according to any one of claims 1 to 3, wherein the electrode coating layer is obtained by spraying powder containing a positive electrode main material and a conductive agent into the inside or on the surface of a support by a sputtering technique.
5. The positive electrode plate of the lithium ion secondary battery as claimed in claim 4, wherein the powder is obtained by kneading a positive electrode main material and a conductive agent by a high-speed dispersion device; the linear speed of the mashup is controlled to be 25-60 m/s.
6. The positive electrode sheet for a lithium-ion secondary battery according to claim 5, wherein the sputtering direction is perpendicular to the surface of the support, and the sputtering speed is 5 to 30 m/s.
Preferably, the distance between the sputtering nozzle and the carrier is 40-100 mm.
7. The positive electrode plate of the lithium ion secondary battery as claimed in any one of claims 4 to 6, wherein the temperature of the carrier is controlled to be 110-120 ℃ before the sputtering.
8. The positive electrode sheet for a lithium ion secondary battery according to any one of claims 4 to 6, wherein the carrier is in a negative pressure environment during the sputtering; the negative pressure interval is controlled to be-0.085 to 0 MPa.
9. The method for preparing the positive electrode plate of the lithium ion secondary battery according to any one of claims 1 to 8, which comprises the steps of laminating an electrode coating, a metal foil and an electrode coating in order to obtain a large electrode plate; the lamination is realized by hot pressing and electromagnetic induction heating processes.
10. The method for preparing the positive electrode plate of the lithium-ion secondary battery as claimed in claim 9, wherein the surface density of the electrode coating is 190g/m and 170-2The metal foil is an 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 25-45 s; the electromagnetic induction heating conditions are as follows: the power is 30-60KW, and the time is 15-18 s.
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| US20140295299A1 (en) * | 2013-03-26 | 2014-10-02 | Kabushiki Kaisha Toshiba | Nonaqueous electrolyte air battery |
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