CN110729441A - MXene/polyimide composite battery diaphragm and preparation method and application thereof - Google Patents
MXene/polyimide composite battery diaphragm and preparation method and application thereof Download PDFInfo
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- CN110729441A CN110729441A CN201910986932.0A CN201910986932A CN110729441A CN 110729441 A CN110729441 A CN 110729441A CN 201910986932 A CN201910986932 A CN 201910986932A CN 110729441 A CN110729441 A CN 110729441A
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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
- H01M50/431—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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
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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
- H01M50/411—Organic 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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Abstract
The invention belongs to the technical field of lithium ion batteries, and discloses an MXene/polyimide composite battery diaphragm and a preparation method and application thereof. Adding MAX phase ceramic into acid liquor, and stirring and reacting at 30-70 ℃ to obtain MXene material; adding the MXene material into deionized water, and performing ultrasonic treatment for 1-9h to obtain a few-layer MXene material; and finally, uniformly coating a small layer of MXene material on a polyimide film, and drying the polyimide film in vacuum to obtain the MXene material. The film has excellent mechanical property, high heat resistance coefficient and high transmittance, can be applied to high-power and quick-charging lithium ion battery diaphragm materials, and finally realizes the application in high-power/quick-charging lithium ion battery diaphragms.
Description
Technical Field
The invention belongs to the technical field of high-performance/high-energy-density lithium ion battery diaphragms, and particularly relates to an MXene/polyimide composite battery diaphragm and a preparation method and application thereof.
Background
During the past decades, lithium ion batteries have received great attention due to their high energy density, light weight and good cycling performance. At present, lithium ion batteries have become commercialized batteries and appear in the aspects of life of people, but the safety problem is always an important problem to be solved urgently by lithium ion batteries. The commonly used lithium ion battery diaphragm is a traditional polypropylene diaphragm, and lithium dendrite can be generated on a lithium negative electrode in the charging and discharging processes, the polypropylene diaphragm can be punctured, the battery is short-circuited, and even the battery can be ignited in severe cases. Meanwhile, the structure of polypropylene is damaged at 80 ℃, so that the holes of the diaphragm are closed, the battery is difficult to continue to use, and the application of the lithium ion battery is greatly limited due to the problems.
Polyimide (PI) has good thermal stability, chemical stability and outstanding mechanical property, the long-term service temperature of the PI can reach 300 ℃, and the PI is a film type insulating material with the best comprehensive performance at present. Compared with polyolefin separators, PI has a polar group and thus has better lithium ion electrolyte affinity, and is therefore considered as a next-generation lithium ion battery separator material.
Two-dimensional materials have attracted considerable attention since their discovery. In 2011, a new member MXene material is added to a two-dimensional material family. Similar to graphene, MXene material has a layered two-dimensional structure, a large specific surface area, extremely high conductivity, excellent mechanical properties and excellent electrical properties. The MXene material is coated on the PI film to be used as the diaphragm material of the lithium ion battery, so that the mechanical property of the diaphragm can be improved, the conductivity of the diaphragm can be improved, the service life of the diaphragm can be prolonged, the MXene material with high specific surface area can also adsorb active substances in the charging and discharging processes, the shuttle of the active substances is avoided, the volume expansion of the electrode material is reduced, and the stability and the safety of the lithium ion battery are improved.
Disclosure of Invention
In order to solve the defects and shortcomings of the traditional battery diaphragm in the prior art in the application of the high-performance/high-energy-density lithium ion battery, the invention mainly aims to provide a preparation method of an MXene/polyimide composite battery diaphragm; the method has simple preparation process and environment-friendly preparation method.
The invention also aims to provide the MXene/polyimide composite battery diaphragm prepared by the preparation method; the composite battery diaphragm has excellent mechanical property, high heat resistance and puncture resistance, can break through the bottleneck of low energy density of lithium ion batteries in the current market, and greatly improves the use safety of products. The lithium ion battery can be used in high/low temperature environments, and can bear the over-high temperature and the growth of lithium dendrites in the charging and discharging process of the battery, so that the cycling stability is improved, the rate capability is improved, and the potential safety hazard caused by over-high temperature is reduced.
The invention further aims to provide application of the MXene/polyimide composite battery diaphragm.
The purpose of the invention is realized by the following technical scheme:
an MXene/polyimide composite battery diaphragm is prepared by adding MAX phase ceramic into acid liquor, and stirring at 30-70 deg.C for reaction to obtain MXene material; adding the MXene material into deionized water, and performing ultrasonic treatment for 1-9 hours to obtain a few-layer MXene material; and finally, uniformly coating a small layer of MXene material on a polyimide film, and drying the polyimide film in vacuum to obtain the MXene material.
Preferably, the MAX phase ceramic is Ti2AlC、Mo2AlC、Cr2AlC、Ti3AlC2、Nb4AlC3、V4AlC3、Mo4AlC3And Ta4AlC3One kind of (1).
Preferably, the liquid acid is hydrofluoric acid; the volume ratio of the MAX phase ceramic to the hydrofluoric acid is 1 g: (5-40) ml.
Preferably, the number of layers of the small-layer MXene material is less than 20.
Preferably, the coating is spray coating by a spray gun or coating by a coating machine or directly pumping and filtering a few layers of MXene materials onto the polyimide film; the mass ratio of the few-layer MXene material to the polyimide film is (0.001-0.5): 1.
preferably, the polyimide diaphragm is prepared by adopting electrostatic spinning or pore-forming by adopting other methods.
Preferably, the thickness range of the MXene/polyimide composite battery diaphragm is 10-50 μm, wherein the thickness range of the polyimide film is 9.9-45 μm, and the thickness of the MXene layer is 0.1-5 μm.
The preparation method of the MXene/polyimide composite battery diaphragm comprises the following specific steps:
s1: adding MAX phase ceramic into acid liquor, and stirring and reacting at 30-70 ℃ to obtain MXene material;
s2: adding the MXene material into deionized water, and performing ultrasonic treatment for 1-9 hours to obtain a few-layer MXene material;
s3: uniformly coating a small layer of MXene material on a polyimide film, and carrying out vacuum drying on the polyimide film to obtain the MXene/polyimide composite battery diaphragm.
Preferably, the stirring reaction time in the step S1 is 10-150 h, and the vacuum drying time in the step S3 is 3-48 h.
The MXene/polyimide composite battery diaphragm is applied to the field of high-heat-resistance lithium ion batteries.
Among the above composite battery separators, the MXene/polyimide composite battery separator has not only high mechanical strength and heat resistance of the polyimide film, but also excellent conductivity and large specific surface area of MXene.
The MXene/polyimide composite battery diaphragm is of a two-layer structure, wherein the polyimide diaphragm at the bottom layer has excellent mechanical property and high heat resistance, so that the material decomposition caused by overhigh local temperature in the charging and discharging processes of the battery is avoided, and the short circuit of the battery caused by the penetration of the diaphragm by the growth of lithium dendrite in the charging and discharging processes can be avoided, thereby improving the cycle stability of the product and enhancing the safety performance of the product. Meanwhile, the MXene material has a large specific surface area, so that the ion transmission can be accelerated, the reduction of the battery capacity due to the shuttling of active substances in the battery charging and discharging process can be avoided, the volume expansion of the active substances can be relieved, the energy density of the product can be further improved, and the bottleneck of the prior art can be broken through. The MXene material and the polyimide are tightly combined, so that the contact resistance between the MXene material and the polyimide can be reduced, the MXene material and the polyimide have good chemical stability and excellent mechanical properties. Therefore, the MXene/polyimide composite diaphragm prepared by the technical scheme has excellent transmission and heat resistance, and can realize high-end application of high-performance/high-energy-density lithium ion battery products.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the MXene/polyimide composite battery diaphragm has excellent mechanical property, high heat resistance and large specific surface area, and can break through the bottleneck of low energy density of lithium ion batteries in the current market; the MXene/polyimide composite battery diaphragm can avoid the penetration of lithium dendrite growth through the diaphragm, and reduce the shuttling of active substances in the charging and discharging process, thereby improving the cycle stability, enhancing the rate capability and reducing the potential safety hazard caused by overhigh temperature.
(2) The polyimide diaphragm in the MXene/polyimide composite battery diaphragm has good mechanical property and high heat resistance, so that the cycling stability and the use safety of the battery are improved.
(3) The MXene in the MXene/polyimide composite battery diaphragm has excellent conductivity and large specific surface area, and reduces shuttling of active substances and volume expansion of the active substances in the charge and discharge processes, thereby improving the battery capacity and the cycling stability.
(4) The MXene/polyimide composite battery diaphragm provided by the invention has the advantages of good ion transmission, excellent mechanical property and high stability, solves the technical defects of poor heat resistance, easy puncture, low discharge rate, low safety and the like of a lithium ion battery diaphragm in the prior lithium ion battery, can be applied to high-power and quick-charge lithium ion battery diaphragm materials, and finally realizes the application of the high-power/quick-charge lithium ion battery diaphragm.
Drawings
Fig. 1 is a charge-discharge cycle curve of the MXene/polyimide (MXene/PI) composite battery separator in example 1.
Fig. 2 is a rate performance curve of the MXene/polyimide (MXene/PI) composite battery separator in example 2.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Weighing 1g of Ti3AlC2Adding the materials into a polytetrafluoroethylene reaction kettle, adding 20ml of hydrofluoric acid, stirring and reacting for 24 hours at 40 ℃, and washing to obtain Ti3C2A material.
(2) Mixing Ti3C2Dissolving the material in water, and performing ultrasonic treatment for 8h to obtain less than 5 layers of Ti3C2A material.
(3) Taking 0.5g of less-layer Ti3C2Adding the materials into a spray gun, uniformly spraying the materials on a Polyimide (PI) diaphragm obtained by 10g of electrostatic spinning, and carrying out vacuum drying for 24h to obtain the MXene/PI composite battery diaphragm.
The MXene/PI composite battery diaphragm replaces a common PP diaphragm to serve as a lithium ion battery diaphragm, metal lithium is adopted as a negative electrode, a commercial 811 electrode is used as a positive electrode, and the electrochemical performance is tested.
FIG. 1 is a cycle curve of the MXene/PI composite battery separator at 0.5A/g in example 1. From fig. 1, it can be seen that the electrochemical performance of a common PP separator rapidly decreases with the increase of the charging and discharging times, and the MXene/PI composite battery separator has good stability, thereby effectively slowing down the decrease of the battery capacity, improving the cycling stability of the battery, and increasing the battery capacity.
Example 2
(1) Weighing 3g V4AlC3Adding the materials into a polytetrafluoroethylene reaction kettle, adding 20ml of hydrofluoric acid, stirring and reacting for 68h at 65 ℃, and washing to obtain V4C3A material.
(2) Will V4C3Dissolving the material in water, and performing ultrasonic treatment for 2h to obtain few layers V less than 54C3A material.
(3) 2g of few layers V are taken4C3Adding the materials into a spray gun, uniformly spraying the materials on a Polyimide (PI) diaphragm obtained by 20g of electrostatic spinning, and carrying out vacuum drying for 36h to obtain the MXene/PI composite battery diaphragm.
The MXene/PI composite battery diaphragm replaces a common PP diaphragm to serve as a lithium ion battery diaphragm, metal lithium is adopted as a negative electrode, a commercial 811 electrode is used as a positive electrode, and the electrochemical performance is tested.
FIG. 2 is the rate performance curve of the MXene/PI composite battery diaphragm in example 2. From fig. 2, it can be seen that the electrochemical performance of the common PP separator increases with the current, the capacity decreases rapidly, the MXene/PI composite battery separator has good stability, high capacity under high current, and excellent rate performance.
Example 3
(1) 1.5g of Ta are weighed4AlC3Adding the materials into a polytetrafluoroethylene reaction kettle, adding 30ml of hydrofluoric acid, stirring and reacting for 60 hours at 55 ℃, and washing to obtain Ta4C3A material.
(2) Will V4C3Dissolving the material in water, and performing ultrasonic treatment for 4h to obtain less than 5 layers of Ta4C3A material.
(3) Taking 3g of few layers of Ta4C3Adding the materials into a spray gun, uniformly spraying the materials on a Polyimide (PI) diaphragm obtained by 10g of electrostatic spinning, and carrying out vacuum drying for 48 hours to obtain the MXene/PI composite battery diaphragm.
The MXene/PI composite battery diaphragm replaces a common PP diaphragm to serve as a lithium ion battery diaphragm, the negative electrode adopts metal lithium, the positive electrode adopts a commercial 811 electrode, and the electrochemical performance is tested.
Example 4
(1) Weighing 2g of Ti2Adding AlC material into a polytetrafluoroethylene reaction kettle, adding 50ml of hydrofluoric acid, stirring and reacting for 30h at 30 ℃, and washing to obtain Ti2And C, material.
(2) Mixing Ti2Dissolving the material C in water, and performing ultrasonic treatment for 1h to obtain the product with the concentration of less than5 layers of less Ti2And C, material.
(3) 2g of a small amount of Ti2And adding the material C into a spray gun, uniformly spraying the material C onto a Polyimide (PI) diaphragm obtained by 5g of electrostatic spinning, and carrying out vacuum drying for 24 hours to obtain the MXene/PI composite battery diaphragm.
The MXene/PI composite battery diaphragm replaces a common PP diaphragm to serve as a lithium ion battery diaphragm, the negative electrode adopts metal lithium, the positive electrode adopts a commercial 811 electrode, and the electrochemical performance is tested.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. An MXene/polyimide composite battery diaphragm is characterized in that: adding MAX phase ceramic into acid liquor, stirring and reacting at 30-70 ℃ to obtain MXene material; adding the MXene material into deionized water, and performing ultrasonic treatment for 1-9 hours to obtain a few-layer MXene material; and finally, uniformly coating a small layer of MXene material on a polyimide film, and drying the polyimide film in vacuum to obtain the MXene material.
2. The MXene/polyimide composite battery separator according to claim 1, wherein: the MAX phase ceramic is Ti2AlC、Mo2AlC、Cr2AlC、Ti3AlC2、Nb4AlC3、V4AlC3、Mo4AlC3And Ta4AlC3One kind of (1).
3. The MXene/polyimide composite battery separator according to claim 1, wherein: the liquid acid is hydrofluoric acid; the volume ratio of the MAX phase ceramic to the hydrofluoric acid is 1 g: (5-40) ml.
4. The MXene/polyimide composite battery separator according to claim 1, wherein: the number of the layers of the small-layer MXene material is less than 20.
5. The MXene/polyimide composite battery separator according to claim 1, wherein: the coating is carried out by adopting a spray gun or a coating machine or directly filtering a few layers of MXene materials onto the polyimide film; the mass ratio of the few-layer MXene material to the polyimide film is (0.001-0.5): 1.
6. the MXene/polyimide composite battery separator according to claim 1, wherein: the polyimide diaphragm is prepared by adopting electrostatic spinning or other methods to prepare the porous polyimide diaphragm.
7. The MXene/polyimide composite battery separator according to claim 1, wherein: the thickness range of the MXene/polyimide composite battery diaphragm is 10-50 μm, wherein the thickness range of the polyimide film is 9.9-45 μm, and the thickness of the MXene layer is 0.1-5 μm.
8. The method for preparing MXene/polyimide composite battery separator according to any one of claims 1-7, characterized by comprising the following specific steps:
s1: adding MAX phase ceramic into acid liquor, and stirring and reacting at 30-70 ℃ to obtain MXene material;
s2: adding the MXene material into deionized water, and performing ultrasonic treatment for 1-9 hours to obtain a few-layer MXene material;
s3: uniformly coating a small layer of MXene material on a polyimide film, and carrying out vacuum drying on the polyimide film to obtain the MXene/polyimide composite battery diaphragm.
9. The method of claim 8, wherein: the stirring reaction time in the step S1 is 10-150 hours, and the vacuum drying time in the step S3 is 3-48 hours.
10. Use of the MXene/polyimide composite battery separator as defined in any one of claims 1-7 in the field of high heat resistant lithium ion batteries.
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Cited By (9)
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|---|---|---|---|---|
| CN111554889A (en) * | 2020-04-10 | 2020-08-18 | 上海应用技术大学 | polyimide/MXene composite material and preparation and application thereof |
| CN113411918A (en) * | 2021-06-08 | 2021-09-17 | 合肥工业大学 | High-temperature-resistant Ti in air3C2Composite film heater |
| CN113620295A (en) * | 2021-08-02 | 2021-11-09 | 北京理工大学 | MXene-CoTe composite diaphragm material and preparation method and application thereof |
| CN113851783A (en) * | 2021-09-24 | 2021-12-28 | 山东大学深圳研究院 | MXene-based diaphragm of water-based zinc metal battery and preparation method and application thereof |
| CN113913952A (en) * | 2021-09-29 | 2022-01-11 | 北京航空航天大学 | Polyimide-based electromagnetic shielding film with sandwich structure and preparation method thereof |
| CN114094279A (en) * | 2021-11-02 | 2022-02-25 | 惠州锂威新能源科技有限公司 | Composite diaphragm and preparation method thereof |
| CN114106374A (en) * | 2021-12-28 | 2022-03-01 | 清华大学 | Polyimide-based composite film and preparation method and application thereof |
| CN114142172A (en) * | 2021-12-01 | 2022-03-04 | 远景动力技术(江苏)有限公司 | Functional diaphragm, preparation method thereof and lithium ion battery containing functional diaphragm |
| CN114725380A (en) * | 2022-05-09 | 2022-07-08 | 江苏科技大学 | Self-supporting polyimide @ MXene flexible film and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111554889A (en) * | 2020-04-10 | 2020-08-18 | 上海应用技术大学 | polyimide/MXene composite material and preparation and application thereof |
| CN113411918A (en) * | 2021-06-08 | 2021-09-17 | 合肥工业大学 | High-temperature-resistant Ti in air3C2Composite film heater |
| CN113411918B (en) * | 2021-06-08 | 2022-08-09 | 合肥工业大学 | High-temperature-resistant Ti3C2 composite film heater in air |
| CN113620295A (en) * | 2021-08-02 | 2021-11-09 | 北京理工大学 | MXene-CoTe composite diaphragm material and preparation method and application thereof |
| CN113620295B (en) * | 2021-08-02 | 2022-11-18 | 北京理工大学 | MXene-CoTe composite diaphragm material and preparation method and application thereof |
| CN113851783A (en) * | 2021-09-24 | 2021-12-28 | 山东大学深圳研究院 | MXene-based diaphragm of water-based zinc metal battery and preparation method and application thereof |
| CN113913952A (en) * | 2021-09-29 | 2022-01-11 | 北京航空航天大学 | Polyimide-based electromagnetic shielding film with sandwich structure and preparation method thereof |
| CN114094279A (en) * | 2021-11-02 | 2022-02-25 | 惠州锂威新能源科技有限公司 | Composite diaphragm and preparation method thereof |
| CN114142172A (en) * | 2021-12-01 | 2022-03-04 | 远景动力技术(江苏)有限公司 | Functional diaphragm, preparation method thereof and lithium ion battery containing functional diaphragm |
| CN114142172B (en) * | 2021-12-01 | 2024-04-12 | 远景动力技术(江苏)有限公司 | Functional diaphragm, preparation method thereof and lithium ion battery containing functional diaphragm |
| CN114106374A (en) * | 2021-12-28 | 2022-03-01 | 清华大学 | Polyimide-based composite film and preparation method and application thereof |
| CN114725380A (en) * | 2022-05-09 | 2022-07-08 | 江苏科技大学 | Self-supporting polyimide @ MXene flexible film and preparation method and application thereof |
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Application publication date: 20200124 |