CN113540686A - Functional diaphragm for lithium-sulfur battery and preparation method thereof - Google Patents
Functional diaphragm for lithium-sulfur battery and preparation method thereof Download PDFInfo
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- CN113540686A CN113540686A CN202010312670.2A CN202010312670A CN113540686A CN 113540686 A CN113540686 A CN 113540686A CN 202010312670 A CN202010312670 A CN 202010312670A CN 113540686 A CN113540686 A CN 113540686A
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- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 229920006305 unsaturated polyester Polymers 0.000 claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 239000004020 conductor Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000011230 binding agent Substances 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000000576 coating method Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 229920000098 polyolefin Polymers 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000011247 coating layer Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- -1 polyethylene Polymers 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- SZYJELPVAFJOGJ-UHFFFAOYSA-N trimethylamine hydrochloride Chemical compound Cl.CN(C)C SZYJELPVAFJOGJ-UHFFFAOYSA-N 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052744 lithium Inorganic materials 0.000 abstract description 12
- 229920001021 polysulfide Polymers 0.000 abstract description 7
- 239000005077 polysulfide Substances 0.000 abstract description 7
- 150000008117 polysulfides Polymers 0.000 abstract description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 239000002346 layers by function Substances 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 229910003003 Li-S Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910001216 Li2S Inorganic materials 0.000 description 1
- 229920002319 Poly(methyl acrylate) Polymers 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000120 polyethyl acrylate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
-
- 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
Abstract
The invention discloses a preparation method of a functional diaphragm for a lithium-sulfur battery, which comprises the following steps: coating the first slurry on the positive electrode side of the polyolefin film, drying to form a first coating, coating the second slurry on the first coating and/or the negative electrode side of the polyolefin film, and drying to obtain the functional diaphragm for the lithium-sulfur battery, wherein the method for preparing the first slurry comprises the following steps: adding a dispersing agent into a solvent, stirring to obtain a first liquid, adding a mixture of a carbon conductor and a binder into the first liquid, stirring, and sanding to obtain a first slurry; method of making the second slurry: and adding unsaturated polyester and a pore-forming agent into water to obtain a second liquid, and stirring to obtain a second slurry. By introducing a functional layer on the surface of the polyolefin diaphragm, on one hand, the generation of polysulfide is prevented, and the shuttle effect is avoided; on the other hand, the mechanical property of the diaphragm can be improved, and the puncture strength of the diaphragm is improved, so that the safety of the lithium battery is improved; the lithium ion transmission is promoted, and the multiplying power performance of the battery is improved.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur battery diaphragms, and particularly relates to a functional diaphragm for a lithium-sulfur battery and a preparation method thereof.
Background
Li-S batteries have higher theoretical energy densities, 2654Wh/kg and 2800Wh/L, which are more than five times higher than the theoretical energy density of traditional lithium ion batteries. In addition, the rapid growth of the market is promoted due to the characteristics of abundant and easily available raw materials, low cost and the like of the lithium-sulfur battery.
Li-S batteries produce lithium polysulfides that dissolve in the electrolyte during discharge. Due to the concentration difference, lithium polysulfide diffuses far from the positive electrode to generate a shuttle effect. The "shuttle effect" reduces the utilization, specific capacity and cycling performance of sulfur. At the same time, polysulfide diffuses to the negative electrode, reacts with the lithium negative electrode, causing the battery to self-discharge, and the reaction produces solid-state insulated Li2S and Li2S2Causing deterioration of the surface of the lithium negative electrode and irreversible loss of the active material.
Lithium-sulfur batteries have problems of short cycle life, low rate performance, and poor safety and stability, which are closely related to the characteristics of battery separators. The diaphragm plays an important role in blocking the electronic conductance of positive and negative electrodes in the battery and allowing liquid ions to freely pass through so as to realize the ionic conduction, and is an important determinant factor of the battery, the cycle capacity and the safety performance. The pore structure of the traditional polyolefin lithium battery diaphragm can not effectively prevent lithium polysulfide from shuttling, so that the cycle performance of the battery is reduced, and in addition, crystals formed by lithium ion reduction in the charging and discharging process can pierce the diaphragm, so that the requirement on the anti-piercing capability of the diaphragm is higher.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a preparation method of a functional diaphragm for a lithium-sulfur battery.
The invention also aims to provide the functional diaphragm for the lithium-sulfur battery, which is obtained by the preparation method, and can overcome the defect that the traditional battery diaphragm cannot inhibit the shuttle effect, improve the mechanical property of the diaphragm, improve the puncture strength of the diaphragm, promote ion transmission and improve the ionic conductivity of the diaphragm, thereby improving the safety and rate capability of the lithium battery.
The purpose of the invention is realized by the following technical scheme.
A method of preparing a functional separator for a lithium sulfur battery, comprising: coating the first slurry on the positive electrode side of the polyolefin film, drying to form a first coating layer, coating the second slurry on the first coating layer and/or the negative electrode side of the polyolefin film, drying to form a second coating layer by the dried second slurry, and obtaining the functional diaphragm for the lithium-sulfur battery, wherein,
a method of preparing the first slurry: adding a dispersing agent into a solvent, stirring to obtain a first liquid, adding a mixture of a carbon conductor and a binder into the first liquid, stirring, and sanding to obtain a first slurry;
in the technical scheme, the dispersing agent is one or a mixture of more of polyacrylic acid ammonium salt, trimethylammonium hydrochloride and polyethylene glycol; the carbon conductor is graphene, Super-p or carbon black, and the binder is PVDF (polyvinylidene fluoride) or polyacrylates.
In the above technical scheme, in the method for preparing the first slurry, the solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is (1-20) in parts by mass: 1.
in the above technical scheme, the dispersant is 5 wt% of the solvent.
In the technical scheme, the ratio of the carbon conductor to the binder is (6-70) by mass: (0.5-5).
In the technical scheme, the mixture of the carbon conductor and the binder accounts for 1-25 wt% of the first liquid.
In the technical scheme, the sanding time is 20-60 min.
A method of making the second slurry: adding unsaturated polyester and a pore-forming agent into water to obtain a second liquid, and stirring to obtain a second slurry, wherein the sum of the unsaturated polyester and the pore-forming agent in the second liquid is 3-20 wt%, and the unsaturated polyester is ortho-benzene unsaturated polyester.
In the technical scheme, the ratio of the unsaturated polyester to the pore-forming agent is (10-65) in parts by weight: (0.5 to 3).
In the above technical scheme, the pore-forming agent is polyvinylpyrrolidone or polyethylene glycol.
In the above technical solution, the first slurry and the second slurry are applied by roll coating.
In the technical scheme, the thickness of the first coating is 1-8 μm.
In the technical scheme, the thickness of the second coating is 1-8 μm.
In the technical scheme, the drying temperature is 60-90 ℃, and the drying time is 10-40 s.
In the technical scheme, the stirring time is 10-50 min.
In the above technical scheme, the polyolefin film is a polyethylene film or a polypropylene film.
The functional separator for a lithium-sulfur battery obtained by the above preparation method.
By introducing a functional layer on the surface of the polyolefin diaphragm, on one hand, the generation of polysulfide is prevented, and the shuttle effect is avoided; on the other hand, the mechanical property of the diaphragm can be improved, and the puncture strength of the diaphragm is improved, so that the safety of the lithium battery is improved; the lithium ion transmission is promoted, and the multiplying power performance of the battery is improved.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
The used stirrer is a double-planetary power mixer, and the model is as follows: HY-DLH43L, manufacturer: guangzhou Hongyang mechanical science and technology Co Ltd
The used sanding equipment is a full ceramic nanometer grinder, and the model is as follows: PT-5L, a Producer of Dongguan City Deno mechanical Equipment Co., Ltd
The unsaturated polyester was purchased from: anhuixi New Material science and technology, Inc.
Example 1
A method of preparing a functional separator for a lithium sulfur battery, comprising: and roll coating the first slurry on the positive electrode side of the polyolefin film, drying at 70 ℃ for 30s to form a first coating layer by the first slurry, roll coating a second slurry on the first coating layer, and drying at 70 ℃ for 30s to form a second coating layer by the dried second slurry to obtain the functional diaphragm for the lithium-sulfur battery, wherein the thickness of the first coating layer is 2 mu m, the thickness of the second coating layer is 2 mu m, and the polyolefin film is a polyethylene film.
A method of preparing a first slurry: adding a dispersing agent into a solvent, stirring for 20min by using a stirrer to obtain a first liquid, adding a mixture of a carbon conductor and a binder into the first liquid, stirring for 20min by using the stirrer, and sanding for 20min by using sanding equipment to obtain a first slurry; the solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is 3: 1. the dispersant is polyacrylic acid ammonium salt; the carbon-based conductor is carbon black, and the binder is PVDF (polyvinylidene fluoride). The dispersant accounts for 5 wt% of the solvent, and the ratio of the carbon conductor to the binder is 12: 0.6, the mixture of the carbon-based conductor and the binder was 7 wt% of the first liquid. The carbon-based conductor can form a reduction site for sulfur ions, preventing the generation of polysulfides.
Method of making the second slurry: adding unsaturated polyester and a pore-forming agent into water to obtain a second liquid, stirring for 20min by using a stirrer to obtain a second slurry, wherein the unsaturated polyester is ortho-benzene unsaturated polyester, the pore-forming agent is polyvinylpyrrolidone, the sum of the unsaturated polyester and the pore-forming agent in the second liquid is 4 wt%, and the ratio of the unsaturated polyester to the pore-forming agent is 20: 1. the unsaturated polyester has high mechanical property, can improve the puncture strength of the diaphragm, and meanwhile, the unsaturated polyester has carboxyl, can promote lithium ion transmission and improve the ionic conductivity of the diaphragm.
Example 2
A method of preparing a functional separator for a lithium sulfur battery, comprising: and roll coating the first slurry on the positive electrode side of the polyolefin film, drying at 70 ℃ for 30s to form a first coating layer, roll coating the second slurry on the negative electrode side of the polyolefin film, and drying at 70 ℃ for 30s to form a second coating layer on the dried second slurry, so as to obtain the functional diaphragm for the lithium-sulfur battery, wherein the thickness of the first coating layer is 2.5 mu m, the thickness of the second coating layer is 2 mu m, and the polyolefin film is a polyethylene film.
A method of preparing a first slurry: adding a dispersing agent into a solvent, stirring for 30min by using a stirrer to obtain a first liquid, adding a mixture of a carbon conductor and a binder into the first liquid, stirring for 30min by using the stirrer, and sanding for 36min by using sanding equipment to obtain a first slurry; the solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is 9: 1. the dispersant is trimethyl ammonium hydrochloride; the carbon conductor is graphene, and the binder is polymethyl acrylate. The dispersant accounts for 5 wt% of the solvent, and the ratio of the carbon conductor to the binder is 30: 2.5, the mixture of the carbon-based conductor and the binder is 10 wt% of the first liquid.
Method of making the second slurry: adding unsaturated polyester and a pore-forming agent into water to obtain a second liquid, stirring for 15min by using a stirrer to obtain a second slurry, wherein the unsaturated polyester is o-benzene unsaturated polyester, the pore-forming agent is polyethylene glycol, the sum of the unsaturated polyester and the pore-forming agent in the second liquid is 10 wt%, and the ratio of the unsaturated polyester to the pore-forming agent is 33: 1.
example 3
A method of preparing a functional separator for a lithium sulfur battery, comprising: and roll coating the first slurry on the positive electrode side of the polyolefin film, drying at 70 ℃ for 30s to form a first coating layer, roll coating the second slurry on the first coating layer and the negative electrode side of the polyolefin film, and drying at 70 ℃ for 30s to form a second coating layer from the dried second slurry, so as to obtain the functional diaphragm for the lithium-sulfur battery, wherein the thickness of the first coating layer is 3 mu m, the thickness of the second coating layer is 2 mu m, and the polyolefin film is a polypropylene film.
A method of preparing a first slurry: adding a dispersing agent into a solvent, stirring for 40min by using a stirrer to obtain a first liquid, adding a mixture of a carbon conductor and a binder into the first liquid, stirring for 40min by using the stirrer, and sanding for 40min by using sanding equipment to obtain a first slurry; the solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is 15: 1. the dispersant is polyethylene glycol; the carbon conductor is Super-p, and the adhesive is polyethylacrylate. The dispersant accounts for 5 wt% of the solvent, and the ratio of the carbon conductor to the binder is 10: 3, the mixture of the carbon-based conductor and the binder is 15 wt% of the first liquid.
Method of making the second slurry: adding unsaturated polyester and a pore-forming agent into water to obtain a second liquid, stirring for 30min by using a stirrer to obtain a second slurry, wherein the unsaturated polyester is o-benzene unsaturated polyester, the pore-forming agent is polyethylene glycol, the sum of the unsaturated polyester and the pore-forming agent in the second liquid is 17 wt%, and the ratio of the unsaturated polyester to the pore-forming agent is 50: 1.
the functional separator for lithium sulfur batteries obtained in examples 1 to 3 was tested, and the test results were as follows:
the functional separator for a lithium-sulfur battery obtained in example 1 had a decomposition voltage of 4.8V, a heat shrinkage of 0.7% at 120 ℃ for 1 hour, a puncture strength of 12N, an ionic conductivity: 1.4X 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% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 99.43% after the battery is cycled for 20 circles.
The functional separator for a lithium-sulfur battery obtained in example 2 had a decomposition voltage of 4.7V, a heat shrinkage of 0.8% at 120 ℃ for 1 hour, a puncture strength of 10N, an ionic conductivity: 1.5X 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% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 98.48% after the battery is cycled for 20 circles.
The functional separator for a lithium-sulfur battery obtained in example 3 had a decomposition voltage of 4.7V, a heat shrinkage of 0.9% at 120 ℃ for 1 hour, a puncture strength of 13N, an ionic conductivity: 1.6X 10-3s/cm-1. The sulfur positive electrode and the lithium negative electrode are adopted to assemble the battery, the capacity retention rate is 97% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 97.57% 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 method for preparing a functional separator for a lithium-sulfur battery, comprising: coating the first slurry on the positive electrode side of the polyolefin film, drying to form a first coating layer, coating the second slurry on the negative electrode side of the polyolefin film and/or the first coating layer, and drying to form a second coating layer from the dried second slurry, thereby obtaining the functional separator for the lithium-sulfur battery,
a method of preparing the first slurry: adding a dispersing agent into a solvent, stirring to obtain a first liquid, adding a mixture of a carbon conductor and a binder into the first liquid, stirring, and sanding to obtain a first slurry;
a method of making the second slurry: adding unsaturated polyester and a pore-forming agent into water to obtain a second liquid, and stirring to obtain a second slurry, wherein the sum of the unsaturated polyester and the pore-forming agent in the second liquid is 3-20 wt%.
2. The preparation method according to claim 1, wherein the dispersant is one or more of polyacrylic acid ammonium salt, trimethylammonium hydrochloride and polyethylene glycol, and the unsaturated polyester is an o-benzene type unsaturated polyester.
3. The method of claim 2, wherein the carbon-based conductor is graphene, Super-p, or carbon black.
4. The method of claim 3, wherein the binder is polyvinylidene fluoride or polyacrylate.
5. The preparation method according to claim 4, wherein the pore-forming agent is polyvinylpyrrolidone or polyethylene glycol.
6. The preparation method according to claim 5, wherein the solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is (1-20): 1.
7. the method according to claim 6, wherein the dispersant is 5 wt% of the solvent;
the ratio of the carbon conductor to the binder is (6-70) by mass: (0.5 to 5); the mixture of the carbon-based conductor and the binder accounts for 1-25 wt% of the first liquid.
8. The preparation method of claim 7, wherein the ratio of the unsaturated polyester to the pore-forming agent is (10-65) in parts by mass: (0.5 to 3).
9. The method according to claim 8, wherein the first slurry and the second slurry are applied by roll coating;
the thickness of the first coating is 1-8 mu m; the thickness of the second coating is 1-8 mu m;
the drying temperature is 60-90 ℃, and the drying time is 10-40 s; the stirring time is 10-50 min, and the sanding time is 20-60 min;
the polyolefin film is a polyethylene film or a polypropylene film.
10. The functional separator for a lithium-sulfur battery obtained by the production method according to any one of claims 1 to 9.
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| CN108963153A (en) * | 2018-07-10 | 2018-12-07 | 珠海恩捷新材料科技有限公司 | A kind of lithium ion battery separator and preparation method thereof |
| CN110707264A (en) * | 2019-09-19 | 2020-01-17 | 河北金力新能源科技股份有限公司 | High-conductivity coating diaphragm for lithium-sulfur battery and preparation method and application thereof |
| CN110707266A (en) * | 2019-09-23 | 2020-01-17 | 河北金力新能源科技股份有限公司 | PVDF (polyvinylidene fluoride) mixed coating slurry, preparation method thereof and diaphragm |
| CN110828827A (en) * | 2019-10-18 | 2020-02-21 | 河北金力新能源科技股份有限公司 | High-conductivity slurry, preparation method thereof and diaphragm |
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Application publication date: 20211022 |