CN114156596A - Diaphragm for lithium ion battery and lithium ion battery containing diaphragm - Google Patents

Diaphragm for lithium ion battery and lithium ion battery containing diaphragm Download PDF

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Publication number
CN114156596A
CN114156596A CN202111470986.5A CN202111470986A CN114156596A CN 114156596 A CN114156596 A CN 114156596A CN 202111470986 A CN202111470986 A CN 202111470986A CN 114156596 A CN114156596 A CN 114156596A
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ceramic layer
additive
ceramic
lithium ion
diaphragm
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CN114156596B (en
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汪圣龙
曾凡腾
蒋伟
蒋中林
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Dongguan Mofang New Energy Technology Co ltd
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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
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403—Manufacturing processes of separators, membranes or diaphragms
    • 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
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/411—Organic material
    • H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
    • 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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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Cell Separators (AREA)

Abstract

The invention provides a diaphragm for a lithium ion battery, which comprises a base film, a first ceramic layer and a second ceramic layer, wherein the first ceramic layer contains spherical ceramic particles and a first additive, the spherical ceramic particles and the first additive with a high melting point are mixed to form a compact coating by accumulation on the base film, so that the heat shrinkage rate of the base film can be remarkably reduced, and the heat stability of the diaphragm is improved; the second ceramic layer comprises flaky ceramic particles distributed at intervals and a second additive with a lower melting point, so that on one hand, the second additive can be converted into a molten state to block pores among the flaky ceramic particles when thermal runaway occurs in the battery, so that the lithium ions are prevented from passing through, and further the thermal runaway is effectively controlled; on the other hand, the roughness of the surface of the second ceramic layer, which is in contact with the first ceramic layer, is set between 30nm and 900nm when the flaky ceramic particles and the second additive are mixed for pulping, so that the adhesive force between the first ceramic layer and the second ceramic layer can be better improved, and the overall stability of the diaphragm is improved.

Description

Diaphragm for lithium ion battery and lithium ion battery containing diaphragm
Technical Field
The invention relates to the field of lithium batteries, in particular to a diaphragm for a lithium ion battery and the lithium ion battery containing the diaphragm.
Background
At present, the polyolefin diaphragm has the advantages of strong electrochemical stability, high mechanical strength and the like, and is widely applied to commercial lithium ion battery products. But because the polarity of the polyolefin material is low, the polyolefin material has poor wettability to electrolyte, low liquid retention capacity and poor interface performance; and the polyolefin material has low self-melting point, so that the thermal stability of the diaphragm is poor.
At present, the electrolyte wettability and the thermal stability of the polyolefin diaphragm can be effectively improved by means of ceramic coating and the like on the diaphragm. However, the preparation process of the diaphragm is more complicated by the methods, the diaphragm breaking temperature of the modified diaphragm is still low, and the diaphragm still has the risk of breaking the diaphragm when the temperature reaches 130 ℃, so that the anode and the cathode are in contact with each other to form an internal short circuit, the battery is caused to fire or explode, and the safety risk exists.
In view of the above, it is necessary to provide a technical solution to the above problems.
Disclosure of Invention
One of the objects of the present invention is: the diaphragm for the lithium ion battery is provided to solve the problem of poor thermal stability of the existing diaphragm.
In order to achieve the purpose, the invention adopts the following technical scheme:
a separator for a lithium ion battery, comprising:
a base film;
the first ceramic layer is coated on at least one surface of the base film and comprises spherical ceramic particles and a first additive; the melting point of the first additive is more than or equal to 200 ℃;
the second ceramic layer is coated on one surface, far away from the base film, of the first ceramic layer and comprises flaky ceramic particles and a second additive; the melting point of the second additive is 100-135 ℃;
wherein the roughness of the surface of the second ceramic layer in contact with the first ceramic layer is 30-900 nm.
Preferably, the diameter of the spherical ceramic particles is 0.05-10 μm; the D50 of the flaky ceramic particles is 0.2-10 mu m.
Preferably, the spherical ceramic particles or the flaky ceramic particles are made of at least one of titanium dioxide, silicon dioxide, magnesium oxide, zirconium dioxide, zinc oxide, aluminum oxide, barium sulfate, boehmite, and magnesium hydroxide.
Preferably, the thickness of the first ceramic layer is 1-20 μm; the thickness of the second ceramic layer is 1-30 mu m.
Preferably, the first additive is any one of polyetherimide, polyetheretherketone, polyethersulfone, polyamideimide and polyamic acid.
Preferably, the second additive is any one of polyethylene wax, polyethylene, polymethyl methacrylate and polyvinylpyrrolidone.
Preferably, the ceramic base film further comprises a bonding layer coated between the base film and the first ceramic layer; the thickness of the bonding layer is 1-10 mu m.
Preferably, the bonding layer comprises a bonding agent and an ion conductor, and the mass ratio of the bonding agent to the ion conductor is (0.2-5): (9.8-5).
The invention also provides a lithium ion battery, which comprises a positive plate, a negative plate and a diaphragm arranged between the positive plate and the negative plate, wherein the diaphragm is any one of the diaphragms.
Compared with the prior art, the invention has the beneficial effects that: the diaphragm provided by the invention comprises a first ceramic layer and a second ceramic layer, wherein the first ceramic layer contains spherical ceramic particles and a first additive, and the spherical ceramic particles and the first additive with a high melting point are mixed to be accumulated on a base film to form a compact coating, so that the heat shrinkage rate of the base film can be obviously reduced, and the heat stability of the diaphragm is improved; the second ceramic layer comprises flaky ceramic particles and a second additive with a lower melting point, so that on one hand, the second additive can be converted into a molten state to block pores among the flaky ceramic particles when thermal runaway of the battery occurs, so as to prevent lithium ions from passing through, and further effectively control the thermal runaway; on the other hand, the roughness of the surface of the second ceramic layer, which is in contact with the first ceramic layer, is set between 30nm and 900nm when the flaky ceramic particles and the second additive are mixed for pulping, so that the adhesive force between the first ceramic layer and the second ceramic layer can be better improved, and the overall stability of the diaphragm is improved.
Drawings
Fig. 1 is a schematic structural view of the separator of the present invention.
FIG. 2 is a second schematic structural diagram of the separator of the present invention.
Fig. 3 is a third schematic structural diagram of the separator of the present invention.
In the figure: 1-a base film; 2-a first ceramic layer; 3-a second ceramic layer; 4-adhesive layer.
Detailed Description
The invention provides a diaphragm for a lithium ion battery, which comprises a base film, a first ceramic layer and a second ceramic layer as shown in figures 1-2; the first ceramic layer is coated on at least one surface of the base film and comprises spherical ceramic particles and a first additive; the melting point of the first additive is more than or equal to 200 ℃; the second ceramic layer is coated on one surface, far away from the base film, of the first ceramic layer and comprises flaky ceramic particles and a second additive; the melting point of the second additive is 100-135 ℃; wherein the roughness of the surface of the second ceramic layer in contact with the first ceramic layer is 30-900 nm.
Preferably, the diameter of the spherical ceramic particles is 0.05-10 μm; the D50 of the flaky ceramic particles is 0.2-10 mu m. The flaky ceramic particles arranged at intervals are spread and highly cover the first ceramic layer, and the formation of lithium dendrites can be effectively inhibited.
Preferably, the spherical ceramic particles or the flaky ceramic particles are made of at least one of titanium dioxide, silicon dioxide, magnesium oxide, zirconium dioxide, zinc oxide, aluminum oxide, barium sulfate, boehmite, and magnesium hydroxide.
Preferably, the thickness of the first ceramic layer is 1-20 μm; the thickness of the second ceramic layer is 1-30 mu m. More preferably, the thickness of second ceramic layer is greater than the thickness of first ceramic layer, and the thickness of this kind of structure lamellar granule is great, and its intensity is higher when tiling covers, more can restrain the formation of lithium dendrite, and the spherical granule of first ceramic layer is closely packed, can also provide certain support for the second ceramic layer, and intensity is higher, and the effect of restraining lithium dendrite is better.
Preferably, the first additive is any one of polyetherimide, polyetheretherketone, polyethersulfone, polyamideimide and polyamic acid. By adopting the high-melting-point first additive to be mixed with the spherical ceramic particles, a compact coating can be formed on the base film in an accumulation manner, the heat shrinkage rate of the base film can be remarkably reduced, and the heat stability of the diaphragm is improved. Preferably, the mass ratio of the spherical ceramic particles to the first additive is (6-8): 4-2.
Preferably, the second additive is any one of polyethylene wax, polyethylene, polymethyl methacrylate and polyvinylpyrrolidone. Wherein the mass ratio of the flaky ceramic particles to the second additive is (6-8) to (4-2).
Preferably, the separator further comprises a bonding layer coated between the base film and the first ceramic layer; the thickness of the bonding layer is 1-10 mu m. As shown in fig. 3.
Preferably, the bonding layer comprises a bonding agent and an ion conductor, and the mass ratio of the bonding agent to the ion conductor is (0.2-5): (9.8-5). More preferably, the mass ratio of the binder to the ion conductor is (3-7) to (7-3).
The bonding layer is additionally arranged between the base film and the first ceramic layer, so that on one hand, the bonding force between the base material layer and the first ceramic layer can be improved, and the overall stability of the diaphragm is improved; on the other hand, the bonding layer is also provided with the ion conductor, so that the transmission rate of lithium ions can be effectively improved through the ion conductor, and the influence on the transportation of the lithium ions due to the arrangement of the multilayer diaphragm is avoided.
The invention provides a lithium ion battery, which comprises a positive plate, a negative plate and a diaphragm arranged between the positive plate and the negative plate, wherein the diaphragm is any one of the diaphragms.
The active material layer coated on the positive plate can be of a chemical formula including but not limited to LiaNixCoyMzO2- bNb(wherein a is more than or equal to 0.95 and less than or equal to 1.2, x>0, y is more than or equal to 0, z is more than or equal to 0, and x + y + z is 1,0 is more than or equal to b and less than or equal to 1, M is selected from one or more of Mn and Al, N is selected from one or more of F, P and S), and the positive electrode active material can also be selected from one or more of LiCoO (lithium LiCoO), but not limited to2、LiNiO2、LiVO2、LiCrO2、LiMn2O4、LiCoMnO4、Li2NiMn3O8、LiNi0.5Mn1.5O4、LiCoPO4、LiMnPO4、LiFePO4、LiNiPO4、LiCoFSO4、CuS2、FeS2、MoS2、NiS、TiS2And the like. The positive electrode active material may be further modified, and the method of modifying the positive electrode active material is known to those skilled in the art, for example, the positive electrode active material may be modified by coating, doping, and the like, and the material used in the modification may be one or a combination of more of Al, B, P, Zr, Si, Ti, Ge, Sn, Mg, Ce, W, and the like.
The active material layer coated on the negative electrode sheet can be one or more of graphite, soft carbon, hard carbon, carbon fiber, mesocarbon microbeads, silicon-based materials, tin-based materials, lithium titanate or other metals capable of forming an alloy with lithium. Wherein, the graphite can be selected from one or more of artificial graphite, natural graphite and modified graphite; the silicon-based material can be one or more selected from simple substance silicon, silicon-oxygen compound, silicon-carbon compound and silicon alloy; the tin-based material can be one or more selected from simple substance tin, tin oxide compound and tin alloy.
In order to make the technical solutions and advantages of the present invention clearer, the present invention and its advantages will be described in further detail below with reference to the following detailed description and the accompanying drawings, but the embodiments of the present invention are not limited thereto.
Example 1
A separator for a lithium ion battery comprises a base film, a first ceramic layer and a second ceramic layer; the first ceramic layer is coated on the two surfaces of the base film and comprises spherical ceramic particles and a first additive; the melting point of the first additive is more than or equal to 200 ℃; the second ceramic layer is coated on one surface, far away from the base film, of the first ceramic layer and comprises flaky ceramic particles and a second additive; the melting point of the second additive is 100-135 ℃; wherein the roughness of the surface of the second ceramic layer in contact with the first ceramic layer is 300 nm.
Specifically, the first ceramic layer has a thickness of 10 μm, and the spherical ceramic particles are SiO2The diameter of the spherical ceramic particles is 50-1000 nm, the first additive is polyamide-imide, and the mass ratio of the spherical ceramic particles to the first additive is 7: 3. The second ceramic layer has a thickness of 20 μm and the flaky ceramic particles are Al2O3The second additive is polyethylene wax, and the mass ratio of the flaky ceramic particles to the second additive is 7: 3.
The preparation method of the diaphragm comprises the following steps:
mixing SiO2Mixing and dispersing polyamide-imide, a binder and a dispersing agent in a solvent to obtain first ceramic layer slurry; mixing Al2O3Mixing and dispersing the polyethylene wax binder and the dispersing agent in a solvent to obtain second ceramic layer slurry;
coating the first ceramic layer slurry on one surface of the base film, and drying to obtain a first ceramic layer;
coating the second ceramic layer slurry on the surface, far away from the base film, of the first ceramic layer, wherein the roughness of the surface, in contact with the first ceramic layer, of the second ceramic layer is 300nm, drying to obtain a second ceramic layer, and finishing the preparation of the diaphragm.
Example 2
The difference from example 1 is the structure of the separator. The separator of the present embodiment further includes a bonding layer coated between the base film and the first ceramic layer and having a thickness of 7 μm.
The adhesive layer comprises an adhesive and an ion conductor, and the mass ratio of the adhesive to the ion conductor is 5: 5.
The rest is the same as embodiment 1, and the description is omitted here.
Example 3
Different from embodiment 1, the first additive used in the first ceramic layer is polyetheretherketone.
The rest is the same as embodiment 1, and the description is omitted here.
Example 4
Different from the embodiment 1, the second additive used for the second ceramic layer is polyvinylpyrrolidone in this embodiment.
The rest is the same as embodiment 1, and the description is omitted here.
Example 5
The difference from embodiment 1 is that the second additive used in the second ceramic layer is polymethyl methacrylate.
The rest is the same as embodiment 1, and the description is omitted here.
Example 6
The difference from example 1 is the roughness of the contact surface of the second ceramic layer with the first ceramic layer, which was 800 nm.
The rest is the same as embodiment 1, and the description is omitted here.
Example 7
The difference from example 1 was that the surface of the second ceramic layer in contact with the first ceramic layer had a roughness of 30 nm.
The rest is the same as embodiment 1, and the description is omitted here.
Example 8
Different from example 1, the mass ratio of the spherical ceramic particles to the first additive was 5: 5.
The rest is the same as embodiment 1, and the description is omitted here.
Example 9
Different from example 1, the mass ratio of the spherical ceramic particles to the first additive was 9: 1.
The rest is the same as embodiment 1, and the description is omitted here.
Example 10
Different from example 1, the mass ratio of the flaky ceramic particles to the second additive was 5: 5.
The rest is the same as embodiment 1, and the description is omitted here.
Example 11
Different from example 1, the mass ratio of the flaky ceramic particles to the second additive was 9: 1.
The rest is the same as embodiment 1, and the description is omitted here.
Example 12
Different from example 2, the mass ratio of the spherical ceramic particles to the first additive was 9: 1.
The rest is the same as embodiment 2, and the description is omitted here.
Example 13
Different from example 2, the mass ratio of the flaky ceramic particles to the second additive was 9: 1.
The rest is the same as embodiment 2, and the description is omitted here.
Example 14
The difference from example 2 is the roughness of the contact surface of the second ceramic layer with the first ceramic layer, which was 800 nm.
The rest is the same as embodiment 2, and the description is omitted here.
Example 15
The difference from example 2 is the roughness of the contact surface of the second ceramic layer with the first ceramic layer, which was 30 nm.
The rest is the same as embodiment 2, and the description is omitted here.
Comparative example 1
The difference from example 1 is the structure of the separator. The separator of the present comparative example had a structure of a base film + a ceramic layer, and the ceramic layer included a ceramic material and a binder, that is, a ceramic layer of a conventional separator.
Comparative example 2
The difference from example 1 is the structure of the separator. The first ceramic layer is made of polyethylene wax, and the melting point of the first ceramic layer is 100-135 ℃; the second additive adopted by the second ceramic layer is polyamide-imide, and the melting point is more than 200 ℃.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 3
The difference from example 1 is the structure of the separator. The first additive adopted by the first ceramic layer is polyethylene wax, and the melting point of the first additive is 100-135 ℃.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 4
The difference from example 1 is the structure of the separator. The first ceramic layer is a mixture of flaky ceramic particles and polyamide-imide; the second ceramic layer is formed by spherical ceramic particles and polyethylene wax which are distributed at intervals.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 5
The difference from example 1 is the structure of the separator. The separator structure of this comparative example, which did not have the second ceramic layer, consisted of the base film + the first ceramic layer.
The rest is the same as embodiment 1, and the description is omitted here.
Comparative example 6
The difference from example 1 is the structure of the separator. The separator structure of this comparative example, which did not have the first ceramic layer, consisted of the base film + the second ceramic layer.
The rest is the same as embodiment 1, and the description is omitted here.
The diaphragms prepared in the embodiments 1-15 and the comparative examples 1-6 are applied to lithium ion batteries, and the diaphragms and the corresponding lithium ion batteries obtained are subjected to performance tests, wherein the test results are shown in table 1.
TABLE 1
Figure BDA0003392183700000091
Figure BDA0003392183700000101
The test results show that the diaphragm provided by the invention effectively solves the problem of poor thermal stability of the diaphragm, and simultaneously improves the cycle performance of the lithium ion battery. From the comparison results of examples 1 to 15 and comparative examples 1 to 6, factors affecting the performance of the separator include the type content of the first additive used, the type content of the second additive, the roughness of the contact surface of the second ceramic layer and the first ceramic layer, and the like, and when an appropriate additive is selected and controlled within an appropriate range, the performance of the separator can be improved to be superior.
It can be seen from the comparison between examples 1 and 2 that, after a bonding layer is added between the base film and the first ceramic layer, the thermal shrinkage rate of the battery can be further reduced, and the bonding layer also contains an ion conductor, so that more channels are provided for the migration of lithium ions, and the cycle performance of the battery is improved.
In addition, as can be seen from the comparison of examples 1 and 6 to 7, the higher the roughness of the contact surface of the second ceramic layer and the first ceramic layer, the better the tight bonding degree of the two layers, and the better the improvement of the thermal shrinkage; and if the contact surface of the two is too smooth, the test results show that the improvement of the heat shrinkage rate and the cycle performance is not favorable.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.

Claims (9)

1. A separator for a lithium ion battery, comprising:
a base film;
the first ceramic layer is coated on at least one surface of the base film and comprises spherical ceramic particles and a first additive; the melting point of the first additive is more than or equal to 200 ℃;
the second ceramic layer is coated on one surface, far away from the base film, of the first ceramic layer and comprises flaky ceramic particles and a second additive; the melting point of the second additive is 100-135 ℃;
wherein the roughness of the surface of the second ceramic layer in contact with the first ceramic layer is 30-900 nm.
2. The separator for a lithium ion battery according to claim 1, wherein the spherical ceramic particles have a diameter of 0.05 to 10 μm; the D50 of the flaky ceramic particles is 0.2-10 mu m.
3. The separator for a lithium ion battery according to claim 2, wherein the spherical ceramic particles or the plate-like ceramic particles are made of at least one material selected from the group consisting of titanium dioxide, silicon dioxide, magnesium oxide, zirconium dioxide, zinc oxide, aluminum oxide, barium sulfate, boehmite, and magnesium hydroxide.
4. The separator for a lithium ion battery according to claim 1 or 2, wherein the first ceramic layer has a thickness of 1 to 20 μm; the thickness of the second ceramic layer is 1-30 mu m.
5. The separator for a lithium ion battery according to claim 1, wherein the first additive is any one of polyetherimide, polyetheretherketone, polyethersulfone, polyamideimide, and polyamic acid.
6. The separator for a lithium ion battery according to claim 1, wherein the second additive is any one of polyethylene wax, polyethylene, polymethyl methacrylate, and polyvinylpyrrolidone.
7. The separator according to claim 1, further comprising an adhesive layer coated between the base film and the first ceramic layer; the thickness of the bonding layer is 1-10 mu m.
8. The separator for a lithium ion battery according to claim 7, wherein the adhesive layer comprises a binder and an ion conductor, and the mass ratio of the binder to the ion conductor is (0.2-5): (9.8-5).
9. A lithium ion battery, comprising a positive plate, a negative plate and a diaphragm arranged between the positive plate and the negative plate, wherein the diaphragm is the diaphragm of any one of claims 1 to 8.
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