CN114447271B - Electrode slice preparation method, electrode slice and lithium ion battery - Google Patents
Electrode slice preparation method, electrode slice and lithium ion battery Download PDFInfo
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- CN114447271B CN114447271B CN202111649176.6A CN202111649176A CN114447271B CN 114447271 B CN114447271 B CN 114447271B CN 202111649176 A CN202111649176 A CN 202111649176A CN 114447271 B CN114447271 B CN 114447271B
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011149 active material Substances 0.000 claims abstract description 145
- 238000010521 absorption reaction Methods 0.000 claims abstract description 25
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- 239000007772 electrode material Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 20
- 239000006258 conductive agent Substances 0.000 claims description 18
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- 239000003921 oil Substances 0.000 claims description 16
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- 229910052744 lithium Inorganic materials 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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Classifications
-
- 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
-
- 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
-
- 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
- H01M4/139—Processes of manufacture
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The application relates to the technical field of lithium ion batteries, in particular to a preparation method of an electrode plate, the electrode plate and a lithium ion battery, wherein two active materials with different contact angles are used as raw materials for preparing the electrode plate, capillary holes exist on the obtained electrode plate, and the capillary holes extend from the surface of the electrode plate to the inside of the electrode plate. The electrode plate with the structure is beneficial to the transmission of lithium ions, can improve the porosity of the lithium ion electrode plate under the same compaction density, can obviously reduce the liquid absorption time of the lithium ion electrode plate, further improves the transmission rate of lithium ions and improves the electrical property of a lithium ion battery.
Description
Technical Field
The application relates to the technical field of lithium ion batteries, in particular to a preparation method of an electrode plate, the electrode plate and a lithium ion battery.
Background
Along with the continuous development of science and technology, the application field of lithium ion batteries is expanded to electric automobiles, energy storage power supplies, aviation fields and the like from portable electronic products. Particularly, large-sized electric equipment such as electric automobiles and the like are required to have certain endurance mileage and cycle life matched with the electric automobiles on the premise of ensuring safety, so that higher requirements on the energy density, cycle life and multiplying power performance of the lithium ion battery are provided.
The energy density can be improved in various ways, such as by increasing the thickness of the positive and negative electrode plates, increasing the compacted density of the active material for tight assembly, and increasing the gram capacity of the active material. In contrast, the thickness of the electrode plate is the most direct method for improving the energy density of the battery, compared with the method for improving the compaction density, the method can obviously reduce the use amount of the positive and negative current collectors and the separator, save the material cost, and obviously reduce the process amount of battery production such as coating, drying, compaction, slitting, assembly and the like of the electrode plate, and save the production cost. However, the increase of the thickness of the electrode sheet can cause problems of reduced lithium ion transmission rate and uneven electrolyte infiltration.
The transmission dynamics of the electrode plate is closely related to the microstructure of the electrode plate, the hole structures in the electrode plate and on the surface play an important role in the transmission speed of lithium ions, and particularly under the condition that the thickness of the electrode reaches a certain degree, the problems of the reduction of the transmission speed of the lithium ions and uneven infiltration of electrolyte caused by the increase of the thickness of the electrode plate can be solved by obtaining an ideal hole structure. In the related art, reduced diffusion path length and ohmic resistance can be achieved using 3D microstructured electrodes, resulting in higher capacity and power density. However, 3D microstructured electrodes are relatively expensive and involve additional complex manufacturing steps. In another method, an insoluble organic solvent, i.e., a secondary fluid, is added to the graphite and conductive agent when they are dispersed in an aqueous binder solution, thereby forming a capillary suspension across the sample network, and achieving the effect of producing a highly porous microstructure.
Disclosure of Invention
The application provides a preparation method of an electrode slice, the electrode slice and a lithium ion battery, and aims to solve the problems of complex manufacturing steps, high cost, residual organic solvents and the like existing in the conventional method for changing the pore structure of the electrode slice.
In a first aspect, the present application also provides a method for preparing an electrode sheet, where the electrode sheet is prepared using a first active material and a second active material as raw materials, the contact angle of the first active material is θ 1, and the contact angle of the second active material is θ 2, where θ 1≤40°,50°≤θ2 is greater than 0 ° and less than or equal to 90 °.
In the scheme, the electrode plate is prepared from two active materials with different contact angles, wherein the contact angle theta 1 of the first active material is larger than 0 DEG and smaller than or equal to 40 DEG, the contact angle theta 2 of the second active material is larger than or equal to 50 DEG and smaller than or equal to 90 DEG, the two active materials are mixed to obtain the electrode active material, the contact angle of the first active material is small, the wettability is good, when the electrode plate is prepared, the first active material is preferentially infiltrated by a solvent, the contact angle of the second active material is large, the interfacial tension is large, when the electrode plate is prepared, liquid drops surrounded by particle clusters can be formed, a liquid bridging network is formed by the liquid bridging network and the first active material, and the porous electrode plate with pores distributed on the surface can be obtained after the suspension slurry with the liquid bridging network structure is coated and dried.
With reference to the first aspect, in a possible embodiment, when the first active material and the second active material are both cathode materials, the oil absorption value of the first active material is 12-20mL/100g, and the oil absorption value of the second active material is 3-10mL/100g; when the first active material and the second active material are both anode materials, the oil absorption value of the first active material is 45-80mL/100g, and the oil absorption value of the second active material is 30-39mL/100g.
With reference to the first aspect, in a possible embodiment, the preparation method comprises a combination of any one or more of batching, coating, drying, rolling.
With reference to the first aspect, in a possible embodiment, the dosing process is specifically to uniformly mix a mixture including the first active material, the second active material, a conductive agent, a binder and a solvent.
With reference to the first aspect, in a possible implementation manner, the batching process specifically includes: uniformly mixing the first active material and the second active material to obtain an electrode active material; and uniformly mixing the electrode active material with a conductive agent, an adhesive and a solvent to prepare electrode slurry.
With reference to the first aspect, in one possible embodiment, the contact angle refers to a contact angle between the active material and the solvent.
With reference to the first aspect, in a possible embodiment, the preparation method at least satisfies one of the following features (1) to (4):
(1) The solvent is N-methyl pyrrolidone or water;
(2) The mass percentage of the first active material to the second active material is (10-80): (90-20);
(3) The first active material and the second active material each independently comprise at least one of ternary material, lithium iron phosphate, artificial graphite, natural graphite, silicon oxide and silicon carbon;
(4) The mass ratio of the electrode active material, the conductive agent, the binder and the solvent is 95-99:1-3:0.8-2.0:30-48.
In a second aspect, the present application provides an electrode sheet obtained by using the preparation method of the first aspect, wherein capillary holes exist on the electrode sheet, and at least a part of the capillary holes extend from the surface of the electrode sheet to the inside of the electrode sheet.
In the scheme, capillary holes are formed in the electrode plate, at least one part of the capillary holes can extend from the surface of the electrode plate to the inside of the electrode plate, and the structure is favorable for lithium ion transmission. Under the same compaction density, the porosity of the lithium ion electrode plate can be improved, the liquid absorption time of the lithium ion electrode plate can be obviously reduced, the lithium ion transmission rate can be further improved, and the electrical performance of the lithium ion battery can be improved.
With reference to the second aspect, in a possible embodiment, the capillary holes have a diameter of 1 μm to 8 μm.
With reference to the second aspect, in a possible embodiment, the porosity of the lithium ion electrode sheet is greater than or equal to 35%.
In a third aspect, the present application also provides a lithium ion battery, including the electrode sheet described above or an electrode sheet manufactured by the above manufacturing method.
The technical scheme of the application has at least the following beneficial effects:
The preparation method of the electrode slice provided by the application is characterized in that two active materials with different contact angles are used for preparation, wherein the contact angle theta 1 of the first active material is larger than 0 DEG and smaller than or equal to 40 DEG, the contact angle theta 2 of the second active material is larger than or equal to 50 DEG and smaller than or equal to 90 DEG, the two active materials are mixed to obtain the electrode active material, the contact angle of the first active material is small, the wettability is good, when the electrode slice is prepared, the first active material is preferentially infiltrated by a solvent, the contact angle of the second active material is large, the interfacial tension is large, liquid drops surrounded by particle clusters can be formed when the electrode slice is prepared, a liquid bridging network is formed by the liquid bridging network and the first active material, and the porous electrode slice with capillary pores distributed on the surface can be obtained after the suspension slurry with the liquid bridging network structure is coated and dried.
According to the electrode plate provided by the application, the capillary holes are formed in the electrode plate, and at least a part of the capillary holes can extend from the surface of the electrode plate to the inside of the electrode plate, so that the structure is beneficial to the transmission of lithium ions. Under the same compaction density, the porosity of the lithium ion electrode plate can be improved, the liquid absorption time of the lithium ion electrode plate can be obviously reduced, the lithium ion transmission rate can be further improved, and the electrical performance of the lithium ion battery can be improved.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application as claimed.
Drawings
FIG. 1 is a scanning electron microscope image of an electrode sheet obtained in example 1 of the present application before rolling;
FIG. 2 is a scanning electron microscope image of the electrode sheet obtained in example 1 of the present application after rolling;
FIG. 3 is a scanning electron microscope image of the electrode sheet obtained in comparative example 1 of the present application before rolling;
FIG. 4 is a scanning electron microscope image of the electrode sheet obtained in comparative example 1 of the present application after rolling;
FIG. 5 is a graph showing the pore size distribution of the electrode sheet obtained in example 1 of the present application and comparative example 1;
FIG. 6 is a graph showing the liquid absorption test of the electrode sheet obtained in example 1 of the present application;
FIG. 7 is a graph showing the liquid absorption test of the electrode sheet obtained in comparative example 1 of the present application;
fig. 8 is a graph showing the cycle performance of the full cell prepared from the electrode sheets obtained in example 1 and comparative example 1 according to the present application.
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
Detailed Description
The following description is of the preferred embodiments of the present invention, and it should be noted that, for those skilled in the art, it is possible to make several improvements and modifications without departing from the principle of the embodiments of the present invention, and these improvements and modifications are also considered as the protection scope of the embodiments of the present invention.
In a first aspect, the application provides a method for preparing an electrode sheet, the electrode sheet is prepared by using a first active material and a second active material as raw materials, the contact angle of the first active material is theta 1, the contact angle of the second active material is theta 2, and the theta 1≤40°,50°≤θ2 is more than 0 DEG and less than or equal to 90 deg.
Alternatively, the contact angle θ 1 of the first active material may be 1 °,5 °,8 °, 10 °, 12 °, 15 °,18 °,20 °,25 °, 30 °, 35 °, or 40 °, or the like, but may be other values within the above range, which is not limited herein. The contact angle θ 2 of the second active material may be 50 °, 55 °, 60 °, 65 °, 70 °, 75 °, 80 °, or 90 °, or the like, but may be other values within the above range, and is not limited thereto.
In the scheme, the electrode plate is prepared from two active materials with different contact angles, wherein the contact angle theta 1 of the first active material is larger than 0 DEG and smaller than or equal to 40 DEG, the contact angle theta 2 of the second active material is larger than or equal to 50 DEG and smaller than or equal to 90 DEG, the two active materials are mixed to obtain the electrode active material, the contact angle of the first active material is small, the wettability is good, when the electrode plate is prepared, the first active material is preferentially infiltrated by a solvent, the contact angle of the second active material is large, the interfacial tension is large, when the electrode plate is prepared, liquid drops surrounded by particle clusters can be formed, a liquid bridging network is formed by the liquid bridging network and the first active material, and the porous electrode plate with pores distributed on the surface can be obtained after the suspension slurry with the liquid bridging network structure is coated and dried.
The following describes the present scheme in detail:
With reference to the first aspect, in one possible embodiment, when the first active material and the second active material are both cathode materials, the first active material has an oil absorption value of 12-20mL/100g, such as 12mL/100g, 14mL/100g, 16mL/100g, 18mL/100g, 20mL/100g, and the second active material has an oil absorption value of 3-10mL/100g, such as 3mL/100g, 4mL/100g, 6mL/100g, 8mL/100g, 10mL/100g; when both the first active material and the second active material are anode materials, the oil absorption value of the first active material is 45-80mL/100g, for example 45mL/100g, 50mL/100g, 60mL/100g, 70mL/100g, 80mL/100g, and the oil absorption value of the second active material is 30-39mL/100g, for example 30mL/100g, 32mL/100g, 34mL/100g, 36mL/100g, 39mL/100g.
In the above embodiment, the oil absorption value measuring method includes the steps of:
(a) Weighing a solid powder sample with a certain weight, and placing the solid powder sample into a mixing chamber;
(b) Dropping a solvent (e.g., any one of dibutyl phthalate (DBP), dioctyl phthalate (DOP), linseed oil, deionized water, N-methylpyrrolidone, absolute ethyl alcohol, and acetone) at a constant speed on a solid powder sample and simultaneously stirring with two motor-driven rotary wings;
(c) As the amount of solvent absorbed by the solid powder sample increases, the mixture changes from a free-flowing state to a semi-plastic agglomerate, during which the viscosity of the mixture gradually increases and peaks;
(d) The measurement end point is the weight of the drop solvent when the torque generated by the viscosity characteristic change reaches a set value or reaches a constant percentage of the maximum torque obtained from the torque curve to calculate the oil absorption value (mL/100 g) of the sample to the solvent, and the calculation formula is: d is: oil absorption value, unit is mL/100g; v is: the volume of the solid powder sample absorbing solvent is in mL; m is: the mass of the solid powder sample is expressed in g.
In the above embodiment, the cathode material includes at least one of ternary material, lithium iron phosphate, and the anode material includes at least one of artificial graphite, natural graphite, silicon oxide, and silicon carbon.
In the above embodiments, the oil absorption value of the active material is limited to a certain range, which is more favorable for the full wetting between the active material and the solvent to form capillary pores.
As an alternative embodiment of the present application, the preparation method comprises any one or more of compounding, coating, baking and rolling.
As can be appreciated, in the preparation method, the electrode slurry can be obtained through a batching process, the obtained electrode slurry is transferred to a coater for coating, then dried and finally rolled.
With reference to the first aspect, in a possible implementation manner, the batching process is specifically: the first active material, the second active material, the conductive agent, the adhesive and the solvent are uniformly mixed.
With reference to the first aspect, in a possible implementation manner, the batching process is specifically: uniformly mixing the first active material and the second active material to obtain an electrode active material; and then uniformly mixing the electrode active material with a conductive agent, an adhesive and a solvent to prepare the electrode slurry.
Optionally, the conductive agent may be at least one selected from graphite, carbon black, graphene, carbon nanotube conductive fibers, metal powder, conductive whiskers, conductive metal compounds, and conductive polymers. Specifically, the conductive agent may include ketjen black (ultrafine conductive carbon black having a particle diameter of 30 to 40 nm), SP (Super P, small particle conductive carbon black having a particle diameter of 40 to 50 nm), S-O (ultrafine graphite powder having a particle diameter of 0.5 to 2 μm), KS-6 (large particle graphite powder having a particle diameter of 3 μm), acetylene black, VGCF (vapor grown carbon fiber having a tube diameter of 100 to 300 nm).
Alternatively, the binder may be selected from one of polyvinyl alcohol (PVA), polytetrafluoroethylene (PTFE), sodium carboxymethyl cellulose (CMC), polyolefins (such as PP, PE and other copolymers), polyvinylidene fluoride (PVDF), modified SBR rubber.
Alternatively, the type of solvent may be selected according to the kind of active material, and in particular, the solvent may be selected from N-methylpyrrolidone or water.
Specifically, electrode active materials, a conductive agent and a binder can be mixed in proportion, added into a solvent, and stirred for 5-8 hours by a double-planetary vacuum stirrer at the rotating speed of 800-1200 r/min to obtain electrode slurry.
With reference to the second aspect, in one possible embodiment, the contact angle refers to the contact angle between the active material and the solvent.
It is understood that the contact angle θ 1 is the contact angle between the first active material and the solvent. The contact angle θ 2 is the contact angle between the second active material and the solvent.
With reference to the second aspect, in one possible embodiment, the solvent is N-methylpyrrolidone (NMP) or water.
Alternatively, the water may be deionized water. It is understood that the solvent is N-methylpyrrolidone when the electrode active material is used as a cathode active material, and water when the electrode active material is used as an anode active material.
With reference to the second aspect, in some embodiments, the mass percent of the first active material to the second active material is (10-80): (90-20).
In some embodiments, the first active material and the second active material each independently comprise one of ternary materials, lithium iron phosphate, artificial graphite, natural graphite, silica, or silicon carbon.
In some embodiments, the mass ratio of electrode active material, conductive agent, binder, and solvent is 95-99:1-3:0.8-2.0:30-48.
Alternatively, the mass percent of the first active material to the second active material may be 80: 20. 70:30, 60:40, 50:50, 40:60, 30:70, 20:80, or 10:90, etc., although other values within the above ranges are also possible and are not limited thereto. It can be understood that by reasonably selecting the mass percentages of the first active material and the second active material in the electrode active material, the obtained electrode active material and the solvent can form a more stable liquid bridging network structure in the process of preparing the electrode slice, and further the porous electrode slice obtained after the suspension slurry with the liquid bridging network structure is coated and dried has an ideal capillary pore structure.
Optionally, the first active material is one of ternary material, lithium iron phosphate, artificial graphite, natural graphite, silicon oxide or silicon carbon; the second active material is one of ternary material, lithium iron phosphate, artificial graphite, natural graphite, silicon oxide or silicon carbon.
The first active material may be a polycrystalline high nickel ternary material, alternatively, the chemical formula of the polycrystalline high nickel ternary material is Li a1(Nix1Coy1Mnz1)O2-b1Nb1, wherein a1 is more than or equal to 0.95 and less than or equal to 1.2,0.5 and less than x1 is more than or equal to 0 and less than or equal to 1, y1 is more than or equal to 0 and less than 1, x1+y1+z1=1, b1 is more than or equal to 0 and less than or equal to 1, and N b1 is one or more selected from F, P, S, and specifically, the polycrystalline high nickel ternary material may be commercially available NCM622, NCA811 and NCM88. The second active material can be a single crystal high nickel ternary material, and optionally, the chemical formula of the single crystal high nickel ternary material is Lia 2(Nix2Coy2Mnz2)O2-b2Nb2, wherein a2 is more than or equal to 0.95 and less than or equal to 1.2, x2 is more than or equal to 0 and less than 1, y2 is more than or equal to 0 and less than or equal to 1, x2+y2+z2=1, b2 is more than or equal to 0 and less than or equal to 1, and N b2 is one or more than one of F, P, S. In particular, the single crystal high nickel ternary material may be a commercially available NCM622-S, NCM811-S, NCM88-S.
Alternatively, the mass ratio of the electrode active material, the conductive agent, the binder and the solvent may be 95:1:0.8:30, 96:2:1:35, 98:3:1.2:40, or 99:1:2.0:48, or the like, but may be other values within the above range, which is not limited thereto. It can be appreciated that by reasonably selecting the mass ratio of the electrode active material, the conductive agent, the binder and the solvent, a porous electrode slurry having better rheology, more uniform pore distribution and more uniform dispersion can be obtained.
In a second aspect, the present application also provides an electrode sheet obtained by using the preparation method of the first aspect, where capillary holes exist on the electrode sheet, and at least a part of the capillary holes extend from the surface of the electrode sheet to the inside of the electrode sheet.
In the scheme, capillary holes exist on the electrode plate, and the capillary holes can extend from the surface of the electrode plate to the inside of the electrode plate, so that the structure is beneficial to the transmission of lithium ions. Under the same compaction density, the porosity of the lithium ion electrode plate can be improved, the liquid absorption time of the lithium ion electrode plate can be obviously reduced, the lithium ion transmission rate can be further improved, and the electrical performance of the lithium ion battery can be improved.
The following describes the present scheme in detail:
as an alternative embodiment of the present application, the capillary holes have a diameter of 1 μm to 8. Mu.m.
Alternatively, the diameter of the capillary holes may be 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, or the like, but other values within the above range are also possible, and are not limited thereto. It can be understood that when the diameter of the capillary holes is smaller than 1 μm, the diameter of the capillary holes is too small, the improvement of the porosity of the electrode sheet is not obvious, so that the lithium ion transmission rate is not improved, and when the diameter of the capillary holes is larger than 8 μm, the phenomenon of 'foil leakage' may occur, and the prepared battery may generate lithium precipitation, thereby affecting the safety of the battery.
With reference to the second aspect, in one possible embodiment, the porosity of the electrode sheet is greater than or equal to 35%.
Alternatively, the porosity of the electrode sheet may be 35%, 40%, 45%, 50%, 55%, or the like, but may be other values within the above range, which is not limited thereto. It can be understood that the porosity in the range can obviously reduce the imbibition time of the electrode plate, ensure that the imbibition time can be shortened by more than 10%, improve the lithium ion transmission rate and improve the electrical property of the lithium ion battery.
In a third aspect, the application also provides a lithium ion battery, which comprises the electrode slice and the electrode slice prepared by the preparation method.
The following describes embodiments of the present application in more detail. The embodiments of the present application are not limited to the following specific embodiments. The modification can be appropriately performed within the scope of protection.
Example 1
The preparation method of the electrode slice comprises the following steps:
And (3) selecting a polycrystalline high-nickel ternary material LiNi 0.88Co0.06 Mn0.06O2 as a first active material, a single-crystal high-nickel ternary material LiNi 0.88Co0.06 Mn0.06O2 as a second active material, and mixing the first active material and the second active material according to the mass percentage of 70:30 to obtain the electrode active material, wherein the contact angle theta 1 of the first active material and the solvent NMP is 18 degrees, and the contact angle theta 2 of the second active material and the solvent NMP is 82 degrees. Wherein, contact angles θ 1 and θ 2 are tested using an in situ contact angle test method, which is as follows: the liquid sample is automatically dropped out through an injection system, the liquid drop is dropped on the surface of the solid sample, the appearance image of the liquid drop is obtained through a microscope lens and a camera, and then the contact angle of the liquid drop in the image is calculated by using a digital image and mathematical operation. Instrument name: OCA15EC video optical contact angle measuring instrument.
The electrode active material obtained was mixed with a conductive agent SP, a binder PVDF5130, and NMP at 97.0:2.0:1.2:38.8, and a double planetary vacuum stirrer is adopted for proportioning to obtain qualified cathode slurry with the solid content of 72.1 percent and the viscosity of 5600 mPa.s.
Transferring the qualified slurry to a coater for coating and drying to obtain an electrode plate with capillary holes, carrying out scanning electron microscope test on the obtained electrode plate, wherein the test result is shown in figure 1, rolling the electrode plate to obtain an electrode plate with a certain compaction density, and carrying out scanning electron microscope test on the obtained electrode plate, and the test result is shown in figure 2.
Example 2
In comparison with example 1, example 1 was repeated except that the contact angle θ 1 of the first active material with the solvent NMP in the electrode active material was 1 °, and the contact angle θ 2 of the second active material with the solvent was 90 °.
Example 3
In comparison with example 1, example 1 was repeated except that the contact angle θ 1 of the first active material with the solvent NMP was 40 ° and the contact angle θ 2 of the second active material with the solvent was 50 °.
Example 4
In comparison with example 1, example 1 was repeated except that the contact angle θ 1 of the first active material with the solvent NMP was 25 ° and the contact angle θ 2 of the second active material with the solvent was 75 °.
Example 5
In comparison with example 1, example 1 was repeated except that the contact angle θ 1 of the first active material with the solvent NMP was 32 ° and the contact angle θ 2 of the second active material with the solvent was 82 °.
Example 6
Example 1 was repeated except that the weight percentage of the first active material to the second active material in the electrode active material was 80:20 as compared with example 1.
Example 7
Example 1 was repeated except that the weight percentage of the first active material to the second active material in the electrode active material was 10:90 as compared with example 1.
Example 8
Example 1 was repeated except that the weight percentage of the first active material to the second active material in the electrode active material was 40:60 as compared with example 1.
Example 9
Compared to example 1, except that the electrode active material was mixed with the conductive agent SP, binder PVDF5130, NMP at 95.0:3.0:2.0:48.0, otherwise as in example 1.
Example 10
The preparation method of the electrode slice comprises the following steps:
And (3) selecting the artificial graphite 1 as a first active material, selecting the artificial graphite 2 as a second active material, and mixing the first active material and the second active material according to the mass percentage of 60:40 to obtain the electrode active material, wherein the contact angle theta 1 of the first active material and the solvent water is 18 degrees, and the contact angle theta 2 of the second active material and the solvent water is 56 degrees.
Mixing the obtained electrode active material with a conductive agent SP, a binder CMC, SBR and deionized water according to the proportion of 97.0:1.0:1.4:1.8:140.0, and a double planetary vacuum stirrer is adopted for proportioning to obtain qualified anode slurry with the solid content of 41.7% and the viscosity of 3100 mpa.s.
And transferring the qualified slurry to a coater for coating, drying and rolling to obtain the electrode slice with certain compaction density.
Comparative example 1
In comparison with example 1, example 1 was repeated except that the electrode active material was the first active material. And (3) carrying out scanning electron microscope test on the electrode plate before rolling, wherein the test result is shown in figure 3, rolling again to obtain the electrode plate with certain compaction density, and carrying out scanning electron microscope test on the obtained electrode plate, and the test result is shown in figure 4.
Comparative example 2
In comparison with example 1, example 1 was repeated except that the electrode active material was the second active material.
Comparative example 3
Example 1 was repeated as in example 1 except that the electrode active material was a second active material and the contact angle of the second active material with the solvent was 95 °.
Comparative example 4
In comparison with example 10, the example 10 was repeated except that the contact angle θ of the second active material was 32 °.
Effect analysis
The electrode sheets obtained in the above examples and comparative examples were subjected to the following performance tests:
1. Pore size distribution test: porosity test method (refer to GB/T21650.1-2008 mercury porosimetry and gas adsorption method for measuring pore size distribution and porosity of solid material, section 1), wherein the instrument name is AutoPore9510 mercury porosimeter, model Micromeritics AutoPore 9510. The test method is as follows:
(1) Sample preparation: drying the sample at a high temperature, wherein the specific temperature and time are selected according to the material characteristics and the customer requirements;
(2) Weighing a sample: 2.25+/-0.05 g of double-sided positive plates, 0.15+/-0.05 g of double-sided negative plates, and cutting the width of the pole pieces to about 10 mm;
(3) Loading a sample: placing the sample into an dilatometer;
(4) Seal dilatometer: sealing on the head grinding mouth sealing glass surface by using an A Pi Songzhen container sealing ester;
(5) Installing an dilatometer and performing low-pressure analysis;
(6) High pressure analysis. And taking out the dilatometer from the low-pressure station port, and installing the dilatometer into a high-pressure bin for high-pressure analysis.
2. Liquid absorption test: the instrument name is pipette P100 (10-100 uL). Rolling the pole piece according to the technological compaction density requirement, and cutting the pole piece into a rectangle with the length of 200mm and the width of 30 mm; sucking the calibrated pipettor into electrolyte (10 uL) and vertically dripping the electrolyte onto the surface of a pole piece, and simultaneously pressing a stopwatch to start timing; and stopping after the electrolyte is completely diffused, and recording the total time as the imbibition time of the pole piece.
3. And (3) testing the cycle performance: matching the electrode plates obtained in the examples 1-9 and the comparative examples 1-3 with a conventional graphite anode plate (prepared from artificial graphite and SP, CMC, SBR according to the ratio of 96.0:1.0:1.4:1.6), and performing battery assembly, liquid injection, formation and capacity division to obtain a battery; matching the electrode plates obtained in the example 10 and the comparative example 4 with a conventional cathode plate (prepared from LiNi 0.88Co0.06 Mn0.06O2 and SP, CNT, PVDF according to the proportion of 97.3:1.0:0.5:1.2), and performing battery assembly, liquid injection, formation and capacity division to obtain a battery; the electrochemical performance of the battery is tested by adopting a new wil 5V6A battery detection cabinet, the voltage range is 3.0-4.2V, the charge-discharge current is 1c, the 1500-week cycle retention rate=1500 th discharge specific capacity/first discharge specific capacity, gram capacity (test parameter) =battery capacity-division capacity/active material weight, and the active material weight comprises the total weight of the first active material and the second active material.
Table 1 comparative examples and comparative examples obtained a comparative table of the basic properties of electrode sheets
Table 2 comparative table of basic performances of full cells prepared from electrode sheets obtained in examples and comparative examples
As can be seen from the experimental results obtained in examples 1 to 10 and comparative examples 1 to 4 of Table 1, in combination with FIG. 5, the electrode sheet prepared by the preparation method of the present application has a porosity of 35% or more and a pore size distribution in the range of 1 μm to 8 μm, whereas the electrode sheet prepared by using a single first active material as an electrode active material has a porosity of 32%, which is significantly lower than the porosity of the electrode sheet of the present application, and a pore size distribution in the range of 0 μm to 1 μm, which is smaller than the pore size distribution range of the electrode sheet of the present application. The porosity of the electrode plate prepared by taking the single second active material as the electrode active material can reach 43.5 percent, which is obviously higher than that of the electrode plate of the application, but the pore size distribution is in the range of 2-15 mu m and is larger than that of the electrode plate of the application, which can cause the phenomenon of foil leakage, and the prepared battery can possibly generate lithium precipitation, thereby influencing the safety of the battery. When the contact angle of the electrode active material selected with the solvent is more than 90 °, the prepared slurry is not good due to the wettability with the solvent, resulting in sedimentation of the slurry. When two kinds of artificial graphite with contact angles in the range of 0-40 degrees and specific contact angle values different are selected to prepare the anode plate, capillary pore phenomenon is not observed in the obtained anode plate, the porosity is obviously lower, the initial effect and the positive gram capacity are lower than those of the embodiment of the application, and the normal-temperature cycle life is shortened. As can be seen from the experimental results of examples 1 to 10 of Table 2, the full cell prepared from the electrode sheet of the present application is excellent in capacity, initial efficiency and cycle performance. As can be seen from the experimental results of example 1 and comparative examples 1 to 3, the full cell capacity, the first efficiency and the cell cycle performance prepared by the electrode sheet of the present application are significantly better than those of the electrode sheet prepared by using a single first active material or a single second active material as the electrode active material, which indicates that the electrode sheet of the present application can effectively improve the electrical performance of the full cell.
As can be seen from the scanning electron microscope diagrams of FIGS. 1 to 4, the electrode sheet obtained in the embodiment 1 of the present application has capillary holes distributed on the surface thereof when not rolled, and the capillary holes are uniformly distributed, so that the capillary holes on the surface of the electrode sheet after rolling are clearly visible. When the electrode sheet obtained in comparative example 1 of the present application was not rolled, no obvious capillary holes were observed on the surface of the electrode sheet, and several capillary holes were visible on the surface of the electrode sheet after rolling, and the number of capillary holes was significantly smaller than that of the electrode sheet obtained in example 1 of the present application.
By subjecting the electrode sheets obtained in example 1 of the present application and comparative example 1 to respective liquid absorption tests, it was found that the liquid had uniformly spread around the electrode sheet obtained in example 1 of the present application at a liquid absorption time of 120s, as shown in fig. 6. Whereas the electrode sheet obtained in comparative example 1 of the present application was still uneven in liquid diffusion at a liquid suction time of 220s, as shown in FIG. 7. Therefore, the electrode active material is adopted to prepare the electrode plate, so that the liquid suction time of the electrode plate can be shortened, the liquid suction speed of the electrode plate can be further improved, the battery capacity is increased, and the cycle life of the battery is prolonged.
As can be seen from the comparison of the cycle performance of the full cell of fig. 8, the full cell prepared by using the electrode sheet of the embodiment of the present application has excellent electrical cycle performance.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (8)
1. A preparation method of an electrode slice is characterized in that the electrode slice is prepared by using a first active material and a second active material as raw materials, wherein the contact angle of the first active material is theta 1, the contact angle theta 1 represents the contact angle between the first active material and a first solvent, the first solvent comprises N-methyl pyrrolidone, the contact angle theta 2 is the contact angle between the second active material and a second solvent, the second solvent comprises N-methyl pyrrolidone, and the contact angle of the second active material is
Theta 2, wherein theta 1≤40°,75°≤θ2 is more than or equal to 18 degrees and less than or equal to 90 degrees;
The preparation method of the electrode slice comprises the following steps of: and uniformly mixing the mixture containing the first active material, the second active material, the conductive agent, the adhesive and the solvent, wherein the porosity of the electrode plate is more than or equal to 35%.
2. The method according to claim 1, wherein when the first active material and the second active material are both cathode materials, the first active material has an oil absorption value of 12 to 20mL/100g, and the second active material has an oil absorption value of 3 to 10mL/100g; when the first active material and the second active material are both anode materials, the oil absorption value of the first active material is 45-80mL/100g, and the oil absorption value of the second active material is 30-39mL/100g.
3. The method of claim 1, further comprising a combination of any one or more of coating, baking, and rolling after the dosing.
4. The preparation method according to claim 1, wherein the batching process comprises the following steps: uniformly mixing the first active material and the second active material to obtain an electrode active material; and uniformly mixing the electrode active material with a conductive agent, an adhesive and a solvent to prepare electrode slurry.
5. The method according to claim 4, wherein the method satisfies at least one of the following characteristics (1) to (3):
(1) The mass percentage of the first active material to the second active material is (10-80): (90-20);
(2) The first active material and the second active material each independently comprise at least one of ternary material, lithium iron phosphate, artificial graphite, natural graphite, silicon oxide and silicon carbon;
(3) The mass ratio of the electrode active material, the conductive agent, the binder and the solvent is 95-99:1-3:0.8-2.0:30-48.
6. An electrode sheet obtained by the production method according to any one of claims 1 to 5, wherein capillary holes exist in the electrode sheet, and at least a part of the capillary holes extend from the surface of the electrode sheet to the inside of the electrode sheet.
7. The electrode sheet of claim 6, wherein the capillary holes have a diameter of 1 μm to 8 μm.
8. A lithium ion battery comprising an electrode sheet produced by the production method according to any one of claims 1 to 5 or an electrode sheet according to any one of claims 6 to 7.
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