CN111211276A - Preparation method and application of large-scale porous aramid microfiber diaphragm - Google Patents
Preparation method and application of large-scale porous aramid microfiber diaphragm Download PDFInfo
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- CN111211276A CN111211276A CN202010069898.3A CN202010069898A CN111211276A CN 111211276 A CN111211276 A CN 111211276A CN 202010069898 A CN202010069898 A CN 202010069898A CN 111211276 A CN111211276 A CN 111211276A
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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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
- D06M13/268—Sulfones
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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
- H01M50/409—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
- H01M50/44—Fibrous material
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
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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
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- 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
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Abstract
A preparation method and application of a large-scale porous aramid microfiber diaphragm belong to the technical field of diaphragm preparation. The invention aims to solve the problems of insufficient strength, low heat-resistant temperature and poor wettability of the diaphragm of the existing lithium ion battery, and the method comprises the following steps: adding the aramid chopped fibers into a dimethyl sulfoxide reaction container filled with potassium hydroxide for soaking; cleaning with pure dimethyl sulfoxide, removing redundant potassium hydroxide, dispersing the pre-oxidized aramid chopped fibers in the dimethyl sulfoxide, and mechanically separating; and (3) performing suction filtration to prepare a membrane by adopting a vacuum suction filtration mode, cleaning after the dimethyl sulfoxide is dried, removing redundant dimethyl sulfoxide, taking down the diaphragm, and compacting. The excellent mechanical property of the aramid microfiber can inhibit the growth of lithium dendrite in the circulation process, prevent the occurrence of short circuit phenomenon caused by the fact that the aramid microfiber pierces a diaphragm, and achieve the purposes of prolonging the service life and improving the safety of the battery.
Description
Technical Field
The invention belongs to the technical field of diaphragm preparation, and particularly relates to a preparation method and application of a large-scale porous aramid microfiber diaphragm.
Background
The lithium ion battery has the characteristics of large capacity, quick charge and discharge, long service life and the like, and is widely applied in the fields of military and civil. As one of the key components in the battery structure, the diaphragm is used for isolating the positive electrode and the negative electrode of the battery and providing a migration channel for lithium ions in the cyclic discharge process, so that the quality of the performance of the diaphragm directly influences the electrochemical performance and the safety use performance of the lithium ion battery. However, the existing polyolefin diaphragm is easy to shrink in size at high temperature, has poor wettability to electrolyte and is easy to puncture by dendrite, so that the use and development of the lithium battery are restricted.
The aramid fiber (poly-p-phenylene terephthalamide) is a high-performance fiber with high strength, high modulus, high temperature resistance, solvent resistance and chemical stability, the decomposition temperature of the aramid fiber is up to 550 ℃, the strength of the aramid fiber exceeds 5GPa, the aramid fiber can stably exist in most organic solutions for a long time, and the aramid fiber has the insulating property of organic matters, so that the aramid fiber is an ideal battery diaphragm material. Although the aramid fiber has many advantages, the aramid fiber is not applied to the lithium ion battery at present, mainly because the aramid fiber non-woven fabric diaphragm cannot meet the requirements of the lithium ion battery on the diaphragm aperture and thickness. Generally, fibers with diameters in a micro-nano scale can be used in batteries, and currently, aramid fibers are mainly prepared by a dry jet wet spinning technology, and the diameters of the obtained fibers are about ten microns. In addition, the diaphragm prepared by directly using the aramid short fiber or the pulp has the problems of low strength, uneven structure and the like. Therefore, how to simply and massively prepare the aramid fiber with the diameter of nanometer or submicron scale is a key problem for preparing the aramid porous battery diaphragm at present.
Disclosure of Invention
The invention aims to solve the problems of insufficient strength, low heat-resistant temperature and poor wettability of the existing lithium ion battery diaphragm, and provides a preparation method and application of a large-scale porous aramid microfiber diaphragm.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a large-scale porous aramid microfiber diaphragm comprises the following specific steps:
the method comprises the following steps: preoxidation process of aramid microfiber:
adding the aramid chopped fibers into a dimethyl sulfoxide reaction container filled with potassium hydroxide, and soaking for 2 days;
step two: stripping aramid microfiber:
cleaning the mixed solution obtained in the first step by using pure dimethyl sulfoxide, removing redundant potassium hydroxide, dispersing the preoxidized aramid chopped fibers from which the redundant potassium hydroxide is removed in the dimethyl sulfoxide, controlling the concentration of the aramid chopped fibers in the dimethyl sulfoxide solvent to be 1-3 wt%, and mechanically separating for 30-60 min at the speed of 8000-12000 r/min;
step three: preparing an aramid microfiber diaphragm:
and (3) performing suction filtration on the mixed solution of the pre-oxidized aramid fiber and the dimethyl sulfoxide obtained in the step two in a vacuum suction filtration mode to prepare a membrane, cleaning the membrane for 3-5 times by using deionized water after the dimethyl sulfoxide is dried, removing redundant dimethyl sulfoxide solvent, taking down the membrane, and compacting the membrane by using a hot press to obtain the aramid microfiber membrane.
The porous aramid microfiber diaphragm is applied to a lithium ion battery.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation of the aramid microfiber with high yield weakens hydrogen bonds and pi-pi conjugation between the microfibers through a pre-oxidation swelling process, so that acting force between the microfibers and the microfibers is loosened, and complete separation of internal microfibers and microfibers is realized through mechanical separation.
(2) The membrane has excellent wettability and mechanical property, and the polar functional group on the surface of the aramid fiber is beneficial to improving the wettability of the membrane material to organic electrolyte. Meanwhile, the excellent mechanical property of the aramid microfiber can inhibit the growth of lithium dendrite in the circulation process, prevent the lithium dendrite from puncturing a diaphragm to cause a short circuit phenomenon, and achieve the purposes of prolonging the service life and improving the safety of the battery.
(3) The size stability of the diaphragm at high temperature and the excellent high-temperature resistance of the aramid fiber avoid the contraction of the diaphragm material caused by the rapid temperature rise of the internal temperature of the battery under the conditions of large-current charging and discharging, eliminate potential safety hazards in the use of the battery and ensure the use safety of the battery under extreme conditions.
Drawings
FIG. 1 is an SEM image of aramid microfibers in step two of example 1;
FIG. 2 is a photograph of the aramid microfiber diaphragm obtained in step three of example 1;
fig. 3 is an SEM image of the aramid microfiber membrane prepared in step three of example 1.
Detailed Description
The technical solution of the present invention is further described below with reference to the drawings and the embodiments, but the present invention is not limited thereto, and modifications or equivalent substitutions may be made to the technical solution of the present invention without departing from the spirit of the technical solution of the present invention, and the technical solution of the present invention is covered by the protection scope of the present invention.
In order to obtain a lithium battery diaphragm material with excellent comprehensive performance, the invention provides a two-step separation mode of pre-oxidation swelling and mechanical stripping through the basic idea of mass production of aramid microfiber, so as to strip the skin and the core of the aramid microfiber and realize the preparation of the aramid microfiber with the size of hundreds of nanometers, and simultaneously, the microfiber is assembled into an aramid porous microfiber diaphragm with a compact structure by adopting a vacuum filtration mode and is applied to a lithium ion battery.
The first embodiment is as follows: the embodiment describes a preparation method of a large-scale porous aramid microfiber diaphragm, which comprises the following specific steps:
the method comprises the following steps: preoxidation process of aramid microfiber:
adding the aramid chopped fibers into a dimethyl sulfoxide reaction container filled with potassium hydroxide, and soaking for 2 days; due to strong basicity of the potassium hydroxide, hydrogen ions of microfibers in the aramid chopped fibers can be captured, and the interaction force among the fiber microfibers is weakened, so that the microfibers are easy to strip in a large scale.
Step two: stripping aramid microfiber:
cleaning the mixed solution obtained in the first step with pure dimethyl sulfoxide, removing redundant potassium hydroxide, dispersing the preoxidized aramid chopped fibers with the redundant potassium hydroxide removed in the dimethyl sulfoxide, controlling the concentration of the aramid chopped fibers in the dimethyl sulfoxide solvent to be 1-3 wt%, and mechanically separating for 30-60 min at the speed of 8000-12000 r/min to obtain stripped aramid microfibers as shown in figure 1, wherein the diameter of the fibers is about 200-300 nm;
step three: preparing an aramid microfiber diaphragm:
and (3) performing suction filtration on the mixed solution of the pre-oxidized aramid fiber and the dimethyl sulfoxide obtained in the step two in a vacuum filtration mode to prepare a membrane, cleaning the membrane for 3-5 times by using deionized water after the dimethyl sulfoxide is dried, removing redundant dimethyl sulfoxide solvent, taking down the membrane, and compacting the membrane by using a hot press to obtain the aramid microfiber membrane. The prepared aramid microfiber membrane is shown in fig. 2, and an SEM photograph of the obtained aramid microfiber membrane is shown in fig. 3.
The second embodiment is as follows: in a specific embodiment, in the first step, the mass ratio of the aramid chopped fibers to the potassium hydroxide is 1: 1 to 1.5; the mass ratio of the aramid chopped fibers to the dimethyl sulfoxide is 1: 10 to 20.
The third concrete implementation mode: in the second step of the preparation method of the large-scale porous aramid microfiber diaphragm, the mass ratio of the pre-oxidized aramid chopped fibers to the dimethyl sulfoxide is 1-3: 100.
the fourth concrete implementation mode: in the third step, in the compacting process, the temperature of the hot pressing plate is 100-300 ℃, and the duration time is 10-60 s.
The fifth concrete implementation mode: an application of the porous aramid microfiber diaphragm obtained in any one of the first to fourth specific embodiments, wherein the porous aramid microfiber diaphragm is used for a lithium ion battery.
Example 1:
a preparation method of a large-scale porous aramid microfiber diaphragm comprises the following steps:
preoxidation of aramid chopped fibers:
5g of aramid chopped fibers are placed in a sealed bottle filled with 95g of dimethyl sulfoxide, 15g of potassium hydroxide is added into the reaction container, and the reaction container is soaked for 2 days. Due to strong basicity of the potassium hydroxide, hydrogen ions of microfibers in the aramid chopped fibers can be captured, and interaction force among the microfibers is weakened. The interaction force between the fiber and the micro-fiber is weakened, so that the micro-fiber is easy to peel off in a large scale.
Secondly, stripping aramid microfiber:
and (4) cleaning the solution prepared in the first step by using pure dimethyl sulfoxide, and removing redundant potassium hydroxide. Dispersing the preoxidized aramid fiber with the redundant potassium hydroxide removed in dimethyl sulfoxide, wherein the mass ratio is 1: 100. mechanically separating at 10000r/min for 30 min. The obtained stripped aramid microfiber is shown in figure 1, and the diameter of the fiber is about 200-300 nm.
Preparation of aramid fiber microfiber diaphragm
And (4) performing suction filtration on the aramid microfiber dimethyl sulfoxide mixed solution prepared in the step two by adopting a vacuum suction filtration mode to prepare a membrane. And (3) after the dimethyl sulfoxide is pumped to dryness, cleaning the pumped membrane for 3 times by using deionized water, and removing the redundant dimethyl sulfoxide solvent. And taking down the diaphragm, compacting the diaphragm by using a hot press, wherein the temperature of the hot press plate is 200 ℃, and the duration is 30 s. And taking out the diaphragm to finish the preparation of the aramid microfiber diaphragm. The prepared aramid microfiber separator is shown in fig. 2, and the SEM photograph of the prepared aramid separator is shown in fig. 3.
Fourthly, assembling and testing the lithium ion battery based on the aramid fiber microfiber diaphragm:
a. preparation of a negative electrode: subjecting LiCoO to condensation4Dispersed with conductive carbon in a 5 wt% solution of polyvinylidene fluoride in N-methylpyrrolidone, LiCoO4: conductive carbon: the mass ratio of polyvinylidene fluoride PVDF is 70: 20: 10. and uniformly coating the dispersion solution on the surface of the aluminum foil. And drying in a vacuum drying box at the temperature of 110 ℃ in a glove box to finish the preparation of the cathode.
b. Assembling the lithium ion battery: the lithium ion battery is assembled into the button battery in a layer-by-layer stacking mode, wherein the first layer is a lithium sheet (the thickness is 0.5 mm); the second layer is an aramid microfiber diaphragm; the third layer is LiCoO4And after a plurality of drops of electrolyte are dripped into the electrode, assembling and pressing the electrode, namely completing the assembly of the lithium ion battery, and testing the electrochemical performance of the battery. The tested performance includes cyclic voltammetry, cyclic stability measurement and rate performance.
The cycle performance of the lithium ion battery using the aramid fiber microfiber diaphragm can still keep stable cycle above 1000 circles, and meanwhile, the battery can still stably work in a high-temperature 100 ℃ environment, which shows that the stability of the battery is obviously improved.
Claims (5)
1. A preparation method of a large-scale porous aramid microfiber diaphragm is characterized by comprising the following steps: the method comprises the following specific steps:
the method comprises the following steps: preoxidation process of aramid microfiber:
adding the aramid chopped fibers into a dimethyl sulfoxide reaction container filled with potassium hydroxide, and soaking for 2 days;
step two: stripping aramid microfiber:
cleaning the mixed solution obtained in the first step by using pure dimethyl sulfoxide, removing redundant potassium hydroxide, dispersing the preoxidized aramid chopped fibers from which the redundant potassium hydroxide is removed in the dimethyl sulfoxide, controlling the concentration of the aramid chopped fibers in the dimethyl sulfoxide solvent to be 1-3 wt%, and mechanically separating for 30-60 min at the speed of 8000-12000 r/min;
step three: preparing an aramid microfiber diaphragm:
and (3) performing suction filtration on the mixed solution of the pre-oxidized aramid fiber and the dimethyl sulfoxide obtained in the step two in a vacuum filtration mode to prepare a membrane, cleaning the membrane for 3-5 times by using deionized water after the dimethyl sulfoxide is dried, removing redundant dimethyl sulfoxide solvent, taking down the membrane, and compacting the membrane by using a hot press to obtain the aramid microfiber membrane.
2. The preparation method of the large-scale porous aramid microfiber diaphragm according to claim 1, wherein the preparation method comprises the following steps: in the first step, the mass ratio of the aramid chopped fibers to the potassium hydroxide is 1: 1 to 1.5; the mass ratio of the aramid chopped fibers to the dimethyl sulfoxide is 1: 10 to 20.
3. The preparation method of the large-scale porous aramid microfiber diaphragm according to claim 1, wherein the preparation method comprises the following steps: in the second step, the mass ratio of the pre-oxidized aramid chopped fibers to the dimethyl sulfoxide is 1-3: 100.
4. the preparation method of the large-scale porous aramid microfiber diaphragm according to claim 1, wherein the preparation method comprises the following steps: in the third step, in the compaction process, the temperature of the hot pressing plate is 100-300 ℃, and the duration time is 10-60 s.
5. The application of the porous aramid microfiber diaphragm obtained by any one of claims 1 to 4 is characterized in that: the porous aramid microfiber diaphragm is used for a lithium ion battery.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113488741A (en) * | 2021-06-07 | 2021-10-08 | 华中科技大学 | Asymmetric diaphragm based on para-aramid, preparation method and application |
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Application publication date: 20200529 |