CN111081951A - Ceramic coated battery separator and method of making same - Google Patents
Ceramic coated battery separator and method of making same Download PDFInfo
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- CN111081951A CN111081951A CN202010021708.0A CN202010021708A CN111081951A CN 111081951 A CN111081951 A CN 111081951A CN 202010021708 A CN202010021708 A CN 202010021708A CN 111081951 A CN111081951 A CN 111081951A
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- boron nitride
- alumina
- ceramic
- battery separator
- nitride powder
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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
- 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
- H01M50/431—Inorganic material
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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
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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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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- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Cell Separators (AREA)
Abstract
The invention discloses a ceramic-coated battery diaphragm and a preparation method thereof; the battery diaphragm comprises a base film and a ceramic coating coated on one side or two sides of the base film, wherein the ceramic coating contains boron nitride powder doped with alumina, and the mass ratio of alumina to boron nitride in the boron nitride powder doped with alumina is 1-12: 1. According to the invention, the boron nitride powder doped with alumina is used as a battery diaphragm coating material, the boron nitride powder doped with alumina is a hybrid boron nitride sheet material formed by embedding alumina into a boron nitride sheet after severe grinding, a bonding effect is generated between the alumina and the boron nitride sheet in the material, more abundant ion transmission pore channels are formed, more positive influence is generated on the transmembrane ion transmission process, the internal resistance of a battery cell is greatly reduced, and the capacitance retention rate and the cycle capacity are improved.
Description
Technical Field
The invention belongs to the field of lithium battery diaphragm materials, and particularly relates to a ceramic-coated battery diaphragm and a preparation method thereof.
Background
Separators are key internal layer components in lithium ion batteries. The key performances of the battery such as capacity, cycle performance, charge-discharge current density, high temperature resistance, high strength, safety guarantee and the like are directly related to the diaphragm.
The lithium ion battery separator which is most used in the market at present is a polyolefin separator or a coating separator which takes the polyolefin separator as a base material. Polyolefin is a non-polar material, and has a large polarity difference with polar electrolyte micromolecules, so that the affinity of a polyolefin diaphragm and electrolyte is insufficient, a large amount of electrolyte is not kept for a long time, and the performance of the battery is greatly influenced. Meanwhile, because the thermal stability of the polyolefin material is poor, the diaphragm in the battery shrinks when being heated to cause the short circuit of the positive electrode and the negative electrode, so that the battery is easy to explode, and the safety problem is caused. The ceramic coating process can solve the defect of poor thermal stability of the polyolefin diaphragm, but the interface compatibility of a single conventional ceramic coating organic and inorganic materials is poor, so that the problem of serious powder falling is often caused, and meanwhile, the thickness of the diaphragm and the internal resistance of the battery are increased, so that the energy density of the battery is reduced, and the cycle capacity is reduced.
Based on the problems faced by the current polyolefin diaphragm and ceramic coating diaphragm, the technical personnel in the field urgently need to develop a diaphragm with an excellent coating, solve the above battery safety problems, ensure the chemical stability of the lithium ion battery, improve the ionic conductivity and the capacitance retention rate, and prolong the cycle life. Boron nitride is a ceramic material with high temperature resistance, no toxicity, high thermal conductivity, corrosion resistance, high insulation and excellent comprehensive performance, and the most common hexagonal boron nitride has a graphite-like layered structure, is in a loose state, has a dielectric constant of 4, has good electrical insulation and excellent thermal conductivity, and is the material with the best thermal conductivity in the ceramic material. It is chemically and mechanically stable to metallic lithium, provides a high degree of electronic insulation, and still provides a stable ion channel when the battery is in operation, thereby achieving stable cycling. Therefore, the boron nitride is taken as the lithium ion battery diaphragm coating material, and is a preferable scheme for solving the problems of poor safety, unstable cycle performance and the like of the diaphragm coated by ceramics such as alumina and the like in the prior art.
For example, patent document with publication number CN 109860477 a discloses a composite diaphragm, in which a composite diaphragm body includes a polymer diaphragm and an inorganic nano material layer, and the inorganic nano material layer adopts hexagonal boron nitride or a mixed material of hexagonal boron nitride and one or more materials of beryllium oxide, aluminum nitride, boron nitride, magnesium oxide, aluminum oxide or silicon nitride. However, the above prior art simply mixes alumina and boron nitride, and alumina and boron nitride cannot interact with each other, so that the improvement effect on the performance of the diaphragm is limited.
Disclosure of Invention
In view of the above, the present invention provides a ceramic-coated battery separator and a preparation method thereof, which can reduce the internal resistance of a battery cell, improve the ionic conductivity, and improve the cycle capacity.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a ceramic-coated battery diaphragm which comprises a base film and a ceramic coating coated on one side or two sides of the base film, wherein the ceramic coating contains boron nitride powder doped with alumina.
As a preferable technical scheme, the mass ratio of the alumina to the boron nitride in the alumina-doped boron nitride powder is 1-12: 1.
As a preferable technical solution, the mass ratio of alumina to boron nitride in the alumina-doped boron nitride powder is 10: 1.
As a preferred technical scheme, the preparation method of the boron nitride powder doped with the alumina comprises the following steps: firstly, dry-mixing and grinding the alumina powder and the boron nitride powder, then preparing the blended powder into 60-90 wt% of high-solid-content aqueous dispersion, and then grinding to obtain the alumina-doped boron nitride powder.
As a preferred technical solution, the boron nitride is hexagonal boron nitride.
Preferably, the particle size of the boron nitride is 0.5-3 μm, and the particle size of the alumina is 30-800 nm.
As a preferred technical scheme, the base film is a polyethylene film, a polypropylene film or a polyethylene and polypropylene composite film with the thickness of 5-40 mu m and the porosity of 30-80%; the thickness of the ceramic coating is 0.5-5 μm.
The invention also provides a preparation method of the ceramic-coated battery diaphragm, which comprises the following steps:
(1) firstly, dry-mixing and grinding alumina powder and boron nitride powder, then preparing 60-90 wt% of high-solid-content aqueous dispersion liquid from the mixed powder, and then grinding to obtain alumina-doped boron nitride powder;
(2) diluting the boron nitride powder doped with alumina prepared in the step (1) to prepare ceramic coating slurry;
(3) conveying the base film into a coating device, and coating by using the ceramic coating slurry prepared in the step (2);
(4) and (4) drying and rolling the battery diaphragm coated in the step (3) to obtain a ceramic-coated battery diaphragm finished product.
The invention has the beneficial effects that:
according to the invention, the boron nitride powder doped with alumina is used as a battery diaphragm coating material, the boron nitride powder doped with alumina is a hybrid boron nitride sheet material formed by embedding alumina into a boron nitride sheet after severe grinding, a bonding effect is generated between the alumina and the boron nitride sheet in the material, more abundant ion transmission pore channels are formed, and more positive influence is generated on the transmembrane ion transmission process, so that the internal resistance of a battery cell is greatly reduced, and the capacity retention rate and the cycle capacity are improved.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 is a photograph of the membrane side of the battery separator prepared in example 1;
fig. 2 is a 0.7C/1C cycle discharge curve of the battery separator (NM9+3) of example 1 and the battery separator (9+3) of comparative example 1.
Detailed Description
The present invention is further described with reference to the following drawings and specific examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
Example 1:
(1) mixing alumina powder and hexagonal boron nitride powder according to the mass ratio of 10:1, grinding for 1h in a planetary ball mill, adding the blended powder into water, introducing a dispersing agent to prepare a 90 wt% high-solid-content aqueous dispersion, and grinding for 2h in a horizontal sand mill to obtain alumina-doped boron nitride powder;
(2) diluting the boron nitride powder doped with the aluminum oxide prepared in the step (1) to 40 wt%, adding a binder and a wetting agent, and uniformly mixing to prepare ceramic coating slurry;
(3) conveying the base film into a coating device, and coating by using the ceramic coating slurry prepared in the step (2);
(4) and (4) drying and rolling the battery diaphragm coated in the step (3) to obtain a ceramic-coated battery diaphragm finished product.
A photograph of the membrane surface of the battery separator prepared in example 1 is shown in fig. 1.
Comparative example 1:
(1) adding alumina powder into water, adding a dispersing agent, an adhesive and a wetting agent at the same time, and uniformly mixing to prepare ceramic coating slurry;
(2) conveying the base film into a coating device, and coating by using the ceramic coating slurry prepared in the step (1);
(3) and (3) drying and rolling the battery diaphragm coated in the step (2) to obtain a ceramic-coated battery diaphragm finished product.
Comparative example 2:
(1) adding boron nitride powder into water, adding a dispersing agent, an adhesive and a wetting agent at the same time, and uniformly mixing to prepare ceramic coating slurry;
(2) conveying the base film into a coating device, and coating by using the ceramic coating slurry prepared in the step (1);
(3) and (3) drying and rolling the battery diaphragm coated in the step (2) to obtain a ceramic-coated battery diaphragm finished product.
Comparative example 3:
(1) mixing alumina powder and hexagonal boron nitride powder according to a mass ratio of 10:1, then adding the mixture into water, simultaneously adding a dispersing agent, an adhesive and a wetting agent, and uniformly mixing to prepare ceramic coating slurry;
(2) conveying the base film into a coating device, and coating by using the ceramic coating slurry prepared in the step (1);
(3) and (3) drying and rolling the battery diaphragm coated in the step (2) to obtain a ceramic-coated battery diaphragm finished product.
The battery separators obtained in example 1 and comparative examples 1 to 3 were subjected to performance tests under the same conditions, and the results are shown in table 1.
TABLE 1 comparative results of battery separator Performance test
From the performance indices of table 1, the battery separator of example 1 is superior to comparative examples 1-3. The insulation resistance value in example 1 was much higher than that in comparative examples 1 to 3, indicating that the interaction of boron nitride and alumina together improved the insulation resistance value.
Fig. 2 is a 0.7C/1C cycle discharge curve of the battery separator (NM9+3) of example 1 and the battery separator (9+3) of comparative example 1, and table 2 is capacitance retention rates of the battery separator (NM9+3) of example 1 and the battery separator (9+3) of comparative example 1, and it can be seen from fig. 2 and table 2 that the battery separator of example 1 is significantly better than that of comparative example 1, the capacity retention rate of comparative example 1 is already less than 40% at 500 cycles, while the capacity retention rate of example 1 is still maintained at 85%, and the cycle performance is excellent.
TABLE 2 comparative examples of capacity retention of battery separators
Table 3 shows the results of the process data of the battery separator (NM9+3) of example 1 and the battery separator (9+3) of comparative example 1, and it can be seen from the data in table 3 that the PPK data of example 1 are better than those of comparative example 1, which indicates that the battery made from the battery separator of example 1 has high liquid retention, small internal resistance of the battery cell, good consistency, highly controllable and reliable manufacturing process, and excellent and stable performance.
TABLE 3 comparison of results of battery separator process data
Table 4 shows the ionic conductivities of the battery separators of example 1 and comparative examples 1 to 3, and from the ionic conductivity performance indicators of table 4, the ionic conductivity of the battery separator of example 1 was much higher than that of comparative examples 1 to 3, indicating that alumina nanoparticles were embedded in the boron nitride sheet layer by the intensive milling process, providing a large number of ion transport channels.
TABLE 4 Battery separator Ionic conductivity
| Item | Unit of | Example 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Alumina/boron nitride | Mass ratio of | 10/1 | 10/0 | 0/10 | 10/1 |
| Ionic conductivity | μS/cm | 50.3 | 33.2 | 37.8 | 40.6 |
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (8)
1. A ceramic-coated battery separator comprising a base film and a ceramic coating applied to one or both sides of the base film, characterized in that: the ceramic coating contains boron nitride powder doped with alumina.
2. The ceramic coated battery separator according to claim 1, wherein: the mass ratio of the alumina to the boron nitride in the alumina-doped boron nitride powder is 1-12: 1.
3. The ceramic coated battery separator according to claim 2, wherein: the mass ratio of the alumina to the boron nitride in the alumina-doped boron nitride powder is 10: 1.
4. The ceramic coated battery separator according to claim 1, 2 or 3, wherein: the preparation method of the boron nitride powder doped with the alumina comprises the following steps: firstly, dry-mixing and grinding the alumina powder and the boron nitride powder, then preparing the blended powder into 60-90 wt% of high-solid-content aqueous dispersion, and then grinding to obtain the alumina-doped boron nitride powder.
5. The ceramic coated battery separator according to claim 4, wherein: the boron nitride is hexagonal boron nitride.
6. The ceramic coated battery separator according to claim 4, wherein: the particle size of the boron nitride is 0.5-3 mu m, and the particle size of the alumina is 30-800 nm.
7. The ceramic coated battery separator according to claim 1, wherein: the base film is a polyethylene film, a polypropylene film or a polyethylene and polypropylene composite film with the thickness of 5-40 mu m and the porosity of 30-80%; the thickness of the ceramic coating is 0.5-5 μm.
8. The method of making a ceramic coated battery separator as claimed in any one of claims 1 to 7, wherein: the method comprises the following steps:
(1) firstly, dry-mixing and grinding alumina powder and boron nitride powder, then preparing 60-90 wt% of high-solid-content aqueous dispersion liquid from the mixed powder, and then grinding to obtain alumina-doped boron nitride powder;
(2) diluting the boron nitride powder doped with alumina prepared in the step (1) to prepare ceramic coating slurry;
(3) conveying the base film into a coating device, and coating by using the ceramic coating slurry prepared in the step (2);
(4) and (4) drying and rolling the battery diaphragm coated in the step (3) to obtain a ceramic-coated battery diaphragm finished product.
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| CN202010021708.0A CN111081951A (en) | 2020-01-09 | 2020-01-09 | Ceramic coated battery separator and method of making same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113563803A (en) * | 2021-08-31 | 2021-10-29 | 昆山捷纳电子材料有限公司 | Polishing solution containing alumina-boron carbide hybrid particles and preparation method thereof |
| CN115224440A (en) * | 2022-08-15 | 2022-10-21 | 广东比沃新能源有限公司 | Ultrathin high-performance composite diaphragm for lithium ion battery and preparation method thereof |
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Cited By (2)
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| CN113563803A (en) * | 2021-08-31 | 2021-10-29 | 昆山捷纳电子材料有限公司 | Polishing solution containing alumina-boron carbide hybrid particles and preparation method thereof |
| CN115224440A (en) * | 2022-08-15 | 2022-10-21 | 广东比沃新能源有限公司 | Ultrathin high-performance composite diaphragm for lithium ion battery and preparation method thereof |
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