CN110828827A - High-conductivity slurry, preparation method thereof and diaphragm - Google Patents
High-conductivity slurry, preparation method thereof and diaphragm Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H—ELECTRICITY
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- 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
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- 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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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- 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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Abstract
The invention discloses high-conductivity slurry, a preparation method thereof and a diaphragm, wherein the preparation method of the high-conductivity slurry comprises the following steps: stirring the first liquid and the second liquid to be uniform, and sanding to obtain the high-conductivity slurry, wherein the preparation method of the first liquid comprises the following steps: uniformly mixing water and ethanol, adding a dispersing agent, and stirring uniformly to obtain a first liquid, wherein the dispersing agent is one or a mixture of more of polyacrylic acid ammonium salt, trimethylammonium hydrochloride and polyethylene glycol; the preparation method of the second liquid comprises the following steps: mixing a carbon conductor, PVP, EDTA and a binder, and stirring the mixture uniformly to obtain a second liquid, wherein the carbon conductor is graphene, Super-p or carbon black, and the binder is PVDF or polyacrylate; according to the invention, the functional layer is introduced to the surface of the polyolefin diaphragm, so that on one hand, the generation of polysulfide is prevented, and the shuttle effect is avoided; on the other hand, the functional layer is introduced to promote the dissociation and transfer effects of lithium ions, so that the ionic conductivity of the diaphragm is effectively improved.
Description
Technical Field
The invention belongs to the technical field of battery diaphragms, and particularly relates to high-conductivity slurry, a preparation method thereof and a diaphragm.
Background
In recent years, lithium-sulfur batteries have been receiving increasing attention as an advanced lithium ion battery. The lithium-sulfur battery, namely the battery with the positive electrode (cathode) being sulfur and the negative electrode (anode) being metal lithium, has the theoretical specific capacity of 1675mAh/g and the theoretical specific energy of 2600 Wh/kg.
The sulfur of the positive electrode is separated from the cyclic S in the discharge process8Lithium polysulphides (Li2Sx, x ═ 8, 6, 4 and 2) were converted into linear structures. In Li2S8、Li2S6、Li2S4And Li2S2Among lithium polysulfides, lithium polysulfides having a high sulfur oxidation number (Li2Sx, usually x)>4) Particularly easily dissolved in a hydrophilic electrolyte. Due to the concentration difference, lithium polysulfide dissolved in the electrolyte diffuses far from the positive electrode, i.e., a "shuttle effect" is generated. The shuttle effect can cause the discharge specific capacity of the lithium-sulfur battery to be reduced and the cycle performance to be poor. The battery performance of the lithium-sulfur battery can be improved only by inhibiting the "shuttling effect" of the polysulfide. Research shows that the 'shuttle effect' of polysulfide can be effectively inhibited by doping conductive high molecular polymer into a sulfur electrode. The conductive high molecular polymer additive has an adsorption effect on polysulfide, and can improve the electrochemical performance of the battery. But the specific gravity of sulfur in the entire electrode is reduced due to the addition of the additive, which affects the energy density of the lithium-sulfur battery. And the conductive high molecular polymer is expensive and high in cost, and is not beneficial to industrial production.
The polyolefin material used in the lithium battery industry at present has excellent performances of stable physical and chemical properties, water resistance, low cost, good mechanical properties, stable electrochemistry and the like, but the characteristics of hydrophobicity, low polarity, low surface energy and the like cause weak interaction between a diaphragm and electrolyte, low ionic conductivity and limit the development of lithium ion batteries.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a highly conductive paste capable of suppressing the "shuttling effect" of polysulfides.
Another object of the present invention is to provide a method for preparing the above-mentioned high-conductivity paste.
It is another object of the present invention to provide a separator based on the above-mentioned high-conductivity paste, which is capable of suppressing the "shuttling effect" of polysulfides without affecting the energy density of the battery.
The purpose of the invention is realized by the following technical scheme.
A preparation method of high-conductivity slurry comprises the following steps:
stirring the first liquid and the second liquid to be uniform, and sanding to obtain the high-conductivity slurry,
the preparation method of the first liquid comprises the following steps: uniformly mixing water and ethanol, adding a dispersing agent, and stirring uniformly to obtain the first liquid, wherein the dispersing agent is one or a mixture of more of polyacrylic acid ammonium salt, trimethylammonium hydrochloride and polyethylene glycol;
the preparation method of the second liquid comprises the following steps: mixing a carbon conductor, PVP, EDTA and a binder, and stirring the mixture uniformly to obtain the second liquid, wherein the carbon conductor is graphene, Super-p or carbon black, and the binder is PVDF (polyvinylidene fluoride) or polyacrylates;
the ratio of the water, the ethanol, the dispersing agent, the carbon conductor, the PVP, the EDTA and the binder is (30-90): (6-10): (0.1-0.5): (1-7): (0.1-0.7): (0.4-1.2): (0.1-0.5).
In the above technical scheme, the time for stirring the first liquid and the second liquid to be uniform is 15-50 min.
In the technical scheme, the time for stirring to be uniform after the dispersing agent is added is 2-10 min.
In the technical scheme, the time for mixing the carbon conductor, PVP, EDTA and the binder and then stirring the mixture uniformly is 10-50 min.
In the technical scheme, the sanding time is 15-60 min.
The high-conductivity slurry obtained by the preparation method.
The diaphragm is obtained by coating the high-conductivity slurry on the positive electrode side of a polyolefin film to obtain a coating and drying the coating.
In the above technical scheme, the polyolefin film is a polyethylene film or a polypropylene film.
In the technical scheme, the coating mode is roll coating.
In the technical scheme, the thickness of the coating is 1-8 microns.
The battery using the separator described above has sulfur as the positive electrode and lithium as the negative electrode.
According to the invention, the functional layer is introduced to the surface of the polyolefin diaphragm, so that on one hand, the generation of polysulfide is prevented, and the shuttle effect is avoided; on the other hand, the functional layer is introduced to promote the dissociation and transfer effects of lithium ions, so that the ionic conductivity of the diaphragm is effectively improved.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
In the following examples, the stirring was carried out using a stirrer, which is a double planetary power mixer, model: HY-DLH43L, manufacturer: guangzhou Hongshang mechanical science and technology, Inc.
The sanding adopts the full ceramic nanometer to grind machine, the model: PT-5L, the manufacturer is a Noo mechanical equipment Co., Ltd.
Example 1
A preparation method of high-conductivity slurry comprises the following steps:
stirring the first liquid and the second liquid for 40min to be uniform, sanding for 60min to obtain high-conductivity slurry, wherein,
the preparation method of the first liquid comprises the following steps: mixing water and ethanol, stirring for 10min to be uniform, adding a dispersing agent, and stirring for 10min to be uniform to obtain a first liquid, wherein the dispersing agent is polyacrylic acid ammonium salt;
the preparation method of the second liquid comprises the following steps: mixing a carbon conductor, PVP, EDTA and a binder, and stirring for 20min to be uniform to obtain a second liquid, wherein the carbon conductor is Super-p, and the binder is PVDF (polyvinylidene fluoride); the carbon-based conductor can form a reduction site for sulfur ions to prevent polysulfide from being generated;
according to the mass parts, the ratio of water, ethanol, dispersant, carbon conductor, PVP, EDTA and binder is 30: 10: 0.1: 1.3: 0.1: 0.4: 0.1.
the high-conductivity slurry of the embodiment is coated on the positive electrode side of a polyolefin film in a roll coating mode to obtain a coating layer with the thickness of 1.3 microns, and the coating layer is dried at 70 ℃ for 0.5min to obtain the separator, wherein the polyolefin film is a polypropylene film.
The decomposition voltage of the separator obtained in example 1 was 4.7V, the thermal shrinkage at 130 ℃ for 1 hour was 1.1%, and the tensile strength was 1550Kg/cm2Ion conductivity: 1.2X 10-3s/cm-1. The sulfur positive electrode and the lithium negative electrode are adopted to assemble the battery, the capacity retention rate is 98.8% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 98.84% after the battery is cycled for 20 circles.
Example 2
A preparation method of high-conductivity slurry comprises the following steps:
stirring the first liquid and the second liquid for 40min to be uniform, sanding for 60min to obtain high-conductivity slurry, wherein,
the preparation method of the first liquid comprises the following steps: mixing water and ethanol, stirring for 5min to be uniform, adding a dispersing agent, and stirring for 10min to be uniform to obtain a first liquid, wherein the dispersing agent is trimethylammonium hydrochloride;
the preparation method of the second liquid comprises the following steps: mixing a carbon conductor, PVP, EDTA and a binder, and stirring for 30min to be uniform to obtain a second liquid, wherein the carbon conductor is carbon black, and the binder is polymethyl acrylate;
according to the mass parts, the ratio of water, ethanol, dispersant, carbon conductor, PVP, EDTA and binder is 80: 10: 0.45: 6.7: 0.68: 1.1: 0.45.
the high-conductivity slurry of the embodiment is coated on the positive electrode side of a polyolefin film in a roll coating mode to obtain a coating layer with the thickness of 2 microns, and the coating layer is dried at 70 ℃ for 0.5min to obtain the separator, wherein the polyolefin film is a polyethylene film.
The decomposition voltage of the separator obtained in example 2 was 4.7V, the thermal shrinkage at 130 ℃ for 1 hour was 1.2%, and the tensile strength was 1620Kg/cm2Ion conductivity: 1.0X 10-3s/cm-1. The sulfur positive electrode and the lithium negative electrode are adopted to assemble the battery, the capacity retention rate is 98.5% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 96.18% after the battery is cycled for 20 circles.
Example 3
A preparation method of high-conductivity slurry comprises the following steps:
stirring the first liquid and the second liquid for 40min to be uniform, sanding for 60min to obtain high-conductivity slurry, wherein,
the preparation method of the first liquid comprises the following steps: mixing water and ethanol, stirring for 5min to uniformity, adding dispersant, and stirring for 10min to uniformity to obtain first liquid, wherein the dispersant is polyethylene glycol;
the preparation method of the second liquid comprises the following steps: mixing a carbon conductor, PVP, EDTA and a binder, and stirring for 40min to be uniform to obtain a second liquid, wherein the carbon conductor is graphene, and the binder is polyethylacrylate;
according to the mass parts, the ratio of water, ethanol, dispersant, carbon conductor, PVP, EDTA and binder is 90: 6: 0.48: 3.8: 0.25: 0.44: 0.25.
the high-conductivity slurry of the embodiment is coated on the positive electrode side of a polyolefin film in a roll coating mode to obtain a coating with the thickness of 4 microns, and the coating is dried at 70 ℃ for 0.5min to obtain the separator, wherein the polyolefin film is a polypropylene film.
The decomposition voltage of the separator obtained in example 3 was 4.7V, the thermal shrinkage at 130 ℃ for 1 hour was 0.9%, the tensile strength was 1650Kg/cm2, and the ionic conductivity was: 1.3X 10-3s/cm-1. The sulfur positive electrode and the lithium negative electrode are adopted to assemble the battery, the capacity retention rate is 99.2% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 99.57% after the battery is cycled for 20 circles.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. A preparation method of high-conductivity slurry is characterized by comprising the following steps:
stirring the first liquid and the second liquid to be uniform, and sanding to obtain the high-conductivity slurry,
the preparation method of the first liquid comprises the following steps: uniformly mixing water and ethanol, adding a dispersing agent, and stirring uniformly to obtain the first liquid, wherein the dispersing agent is one or a mixture of more of polyacrylic acid ammonium salt, trimethylammonium hydrochloride and polyethylene glycol;
the preparation method of the second liquid comprises the following steps: mixing a carbon conductor, PVP, EDTA and a binder, and stirring the mixture uniformly to obtain the second liquid, wherein the carbon conductor is graphene, Super-p or carbon black, and the binder is PVDF or polyacrylate;
the ratio of the water, the ethanol, the dispersing agent, the carbon conductor, the PVP, the EDTA and the binder is (30-90): (6-10): (0.1-0.5): (1-7): (0.1-0.7): (0.4-1.2): (0.1-0.5).
2. The method according to claim 1, wherein the first liquid and the second liquid are stirred until the first liquid and the second liquid are uniform for 15 to 50 min.
3. The preparation method according to claim 1, wherein the time for stirring to be uniform after adding the dispersant is 2 to 10 min.
4. The method according to claim 1, wherein the time for mixing the carbon-based conductor, the PVP, the EDTA and the binder and stirring the mixture until the mixture is uniform is 10 to 50 min.
5. The preparation method according to claim 1, wherein the sanding time is 15-60 min.
6. A high-conductivity paste obtained by the production process according to any one of claims 1 to 5.
7. A separator, wherein the high-conductivity paste according to claim 6 is applied to the positive electrode side of a polyolefin film to obtain a coating layer, and dried to obtain the separator.
8. The separator according to claim 7, wherein the polyolefin film is a polyethylene film or a polypropylene film.
9. The separator according to claim 7, wherein the coating is roll-coated, and the thickness of the coating is 1-8 microns.
10. The battery according to any one of claims 7 to 9, wherein sulfur is a positive electrode and lithium is a negative electrode.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113540686A (en) * | 2020-04-20 | 2021-10-22 | 河北金力新能源科技股份有限公司 | Functional diaphragm for lithium-sulfur battery and preparation method thereof |
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Application publication date: 20200221 |