CN111244366A - Preparation method of lithium-sulfur battery diaphragm based on multilayer aramid nanofibers - Google Patents
Preparation method of lithium-sulfur battery diaphragm based on multilayer aramid nanofibers Download PDFInfo
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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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- 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
- H01M50/409—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
A preparation method of a lithium-sulfur battery diaphragm based on multilayer aramid nanofibers belongs to the technical field of diaphragm preparation. The invention aims to solve the problems that the shuttle phenomenon of the lithium-sulfur battery is serious, the potential safety hazard to the battery exists due to the growth of lithium dendrite and the like at present, and the method comprises the following steps: adding aramid fiber into a sealed dimethyl sulfoxide silk-top bottle, adding potassium hydroxide, and reacting for 2 weeks under magnetic stirring at room temperature; dripping an aramid nano-fiber solution on a rectangular glass sheet, rotating for 30s, simultaneously soaking in deionized water, drying in an oven after dimethyl sulfoxide is completely removed, then soaking a diaphragm in 0.1 wt% of PDDA solution for 30s, taking out, washing redundant PDDA solution, drying in the oven, and sequentially repeating the operations of suspension coating, soaking and suspension coating. The diaphragm prepared by the invention has super-strong mechanical properties (the tensile strength is 165MPa, and the tensile modulus is 9.2GPa), can effectively inhibit the growth of dendrite and ensure the safe use of the battery.
Description
Technical Field
The invention belongs to the technical field of diaphragm preparation, and particularly relates to a preparation method of a lithium-sulfur battery diaphragm based on multilayer aramid nano fibers.
Background
Lithium ion batteries are widely used in the field of people's daily life. With the development of society, the traditional lithium ion battery can not meet the requirement of people on energy storage. Lithium-sulfur batteries (Li-S) are considered to be one of the most promising high-capacity storage systems due to their high theoretical specific capacity and energy density, and the advantages of sulfur, such as low cost and environmental friendliness. However, the commercial application of Li-S batteries still presents some technical challenges, such as the insulating properties of solid sulfides, the shuttling effect of soluble long-chain polysulfides, and the large volume change of sulfur during charging and discharging. These problems often result in low sulfur utilization, poor cycle life, and even a series of safety issues. How to greatly improve the practical energy density and the cycle stability of the Li-S battery has become one of the hot spots of the current research.
During use, polysulphides (LPS, Li)2SXAnd x is more than or equal to 4 and less than or equal to 8) is the biggest problem at present. Shuttling of polysulfides greatly shortens the cycle life of lithium-sulfur batteries and causes the self-discharge phenomenon of the batteries. In addition, after the polysulfide diffuses to the surface of the lithium electrode, the polysulfide reacts with the surface of the lithium electrode, so that the impedance of the battery is significantly increased, and thus energy loss is caused. The separator is one of the important components of the battery, and functions to conduct ion transport and prevent short circuit of the battery. Commercial PP separators, due to their large pore size, allow polysulfides to pass through more easily, and thus cannot effectively inhibit diffusion and shuttling of polysulfides. Therefore, preparing a separator material that can be "ion selective" is currently the most effective method and approach to solve this problem, allowing lithium ions to pass through to ensure normal use of the cell, while hindering the shuttling of polysulfides, preventing their impact on the cell. Meanwhile, the growth of lithium dendrites also needs attention during the use of the battery, mainly because the dendrites can pierce the diaphragm of the battery to cause short circuit of the battery, which also brings about a problemSome potential safety hazard problems.
Disclosure of Invention
The invention aims to solve the problems that the shuttle phenomenon of the conventional lithium-sulfur battery is serious, the potential safety hazard to the battery exists due to the growth of lithium dendrite and the like, and provides a preparation method of a lithium-sulfur battery diaphragm for efficiently inhibiting the shuttle of polysulfide based on multilayer aramid nanofibers.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a lithium-sulfur battery diaphragm based on multilayer aramid nanofibers comprises the following steps:
the method comprises the following steps: preparing an aramid nanofiber solution:
adding aramid fiber into a sealed dimethyl sulfoxide (DMSO) wire-mouth bottle, adding potassium hydroxide, and magnetically stirring at room temperature for reaction for 2 weeks until the aramid fiber is completely dissolved and the solution is dark red, thereby completing the preparation of the aramid nanofiber solution;
step two: preparing a multilayer aramid nanofiber membrane:
dropwise adding the aramid fiber nanofiber solution obtained in the step one onto a rectangular glass sheet, rotating the rectangular glass sheet at a speed of 1500r/min for 30s, simultaneously soaking the rectangular glass sheet into deionized water, standing for 1 day, continuously replacing the deionized water until dimethyl sulfoxide in the solution is completely removed, drying in an oven after the dimethyl sulfoxide in the solution is completely removed, soaking a diaphragm in 0.1 wt% of PDDA solution for 30s, washing the redundant PDDA solution on the surface with the deionized water after the diaphragm is taken out, drying in the oven, and sequentially repeating the operations of suspension coating, soaking and suspension coating to obtain a diaphragm with 5 layers.
Compared with the prior art, the invention has the beneficial effects that: the diaphragm prepared by the invention has super-strong mechanical properties (the tensile strength is 165MPa, and the tensile modulus is 9.2GPa), can effectively inhibit the growth of dendrite and ensure the safe use of the battery. In addition, the small pore diameter of the separator can selectively allow lithium ions to pass through, and simultaneously prevent polysulfides such as LPS from passing through, so that the purpose of ion selectivity is achieved, and the electrochemical stability of the Li-S battery is improved. Due to the super-strong mechanical property and small aperture, the prepared lithium-sulfur battery can be circulated for more than 10000 circles, and the application of the lithium-sulfur battery in various fields is ensured.
Drawings
FIG. 1 is a schematic structural view of a lithium sulfur battery separator prepared according to the present invention;
FIG. 2 is a picture of a multi-layer aramid nanofiber membrane in step two of example 1;
FIG. 3 is a SEM picture of a multilayer aramid nanofiber membrane prepared in step two of example 1;
fig. 4 is a picture of polysulfide shuttle experiment based on multilayer aramid nanofiber membrane in example 1;
fig. 5 is a picture of polysulfide shuttle experiment based on polyolefin membrane in 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.
The first embodiment is as follows: the embodiment describes a method for preparing a lithium-sulfur battery diaphragm based on multilayer aramid nanofibers, which comprises the following steps:
the method comprises the following steps: preparing an aramid nanofiber solution:
adding aramid fiber into a sealed dimethyl sulfoxide (DMSO) wire-mouth bottle, adding potassium hydroxide, and magnetically stirring at room temperature for reaction for 2 weeks until the aramid fiber is completely dissolved and the solution is dark red, thereby completing the preparation of the aramid nanofiber solution;
step two: preparing a multilayer aramid nanofiber membrane:
dropwise adding the aramid fiber nanofiber solution obtained in the step one onto a rectangular glass sheet, rotating the rectangular glass sheet at a speed of 1500r/min for 30s to uniformly coat the aramid fiber nanofiber solution on the surface of the rectangular glass sheet, soaking the rectangular glass sheet into deionized water, and standing for 1 day to realize slow exchange of protons; and continuously replacing deionized water until dimethyl sulfoxide in the solution is completely removed, drying in an oven after the dimethyl sulfoxide in the solution is completely removed, soaking the membrane in 0.1 wt% of PDDA solution for 30s, washing redundant PDDA solution on the surface with the deionized water after the membrane is taken out, drying in the oven, and sequentially repeating the operations of suspension coating, soaking and suspension coating to obtain the 5-layer aramid nano fiber/PDDA/aramid nano fiber membrane. PDDA: poly (diallyldimethylammonium chloride).
The second embodiment is as follows: in a preparation method of a lithium-sulfur battery separator based on multilayer aramid nanofibers, in the first step, the mass ratio of the aramid fibers, dimethyl sulfoxide and potassium hydroxide is 2: 98: 3.
the third concrete implementation mode: in the second step, every 1-5 mL of aramid nano-fiber solution is dripped onto a rectangular glass sheet with the length multiplied by the width of 60-80 mm multiplied by 30-50 mm.
The fourth concrete implementation mode: in a second step of the preparation method of the lithium-sulfur battery separator based on the multilayer aramid nanofibers, the continuous replacement means replacement once every 3 to 5 hours.
The fifth concrete implementation mode: in the second step, the drying temperature is 40-70 ℃ and the drying time is 10-60 min.
Example 1:
a preparation method of a lithium-sulfur battery diaphragm based on multilayer aramid nanofibers comprises the following steps:
step one, preparing an aramid nanofiber solution:
putting 2g of aramid fiber into a sealed bottle filled with 98g of dimethyl sulfoxide, adding 3g of potassium hydroxide into the reaction container, slowly stirring for 2 weeks, slowly dissolving the aramid fiber, and meanwhile, enabling the color of the solution to be deep red, wherein the nano aramid fiber is shown in figure 2, and thus the successful preparation of the nano aramid fiber is proved.
Step two, preparing a multilayer aramid nanofiber membrane:
fixing a rectangular glass sheet with the size of 60mm x 30mm on a suspension coater, and dripping 2mL of the aramid nanofiber solution obtained in the first step into the center of the glass sheet. And (3) rotating the glass sheet at the speed of 1500r/min for 30s to uniformly coat the aramid nano-fiber solution on the surface of the glass. And (3) immersing the glass sheet coated with the aramid nano-fiber solution into 500mL of deionized water to realize solvent replacement, and simultaneously replacing the deionized water every 12h (5 times) to fully remove the dimethyl sulfoxide solvent. After the solvent is replaced, taking out the glass sheet coated with the aramid nano-fiber solution, drying the glass sheet at 60 ℃ for 1h, and soaking the dried glass sheet in 0.1 wt% of poly (diallyldimethylammonium chloride) (PDDA) solution for 30 s. Taking out and washing the excessive PDDA solution on the surface by using deionized water. After the completion, the mixture is transferred to an oven to be dried for 15min at 60 ℃.
And fixing the dried double-layer film glass sheet on a suspension coater again, dripping 2mL of aramid nano-fiber solution into the center of the film, performing suspension coating at 1500r/min for 30s, repeating the operation of soaking and suspension coating in sequence, soaking the obtained diaphragm in ANF, and finally preparing the 5-layer-structured aramid nano-fiber/PDDA/aramid nano-fiber diaphragm. The small pore size of the membrane stacked by nanofibers enables the passage of lithium ions while preventing the shuttling effect of polysulfides. The excellent mechanical property of the aramid nano-fiber ensures the inhibition effect of the diaphragm material on dendrites, and realizes the effect of safety and stability of the battery. A schematic of the preparation of the 5-layer separator is shown in figure 1. The pictures of 5 layers of aramid nanofiber/PDDA membrane are shown in fig. 2 and SEM picture is shown in fig. 3.
And thirdly, comparing the lithium-sulfur battery assembly and shuttle experiments based on the multilayer aramid nanofiber membrane:
a、Li2S6the preparation of (1): in a glove box, Li2And S powder are mixed according to a molar ratio of 1: 5 into a stripping vial with DOL/DME as solvent; the prepared concentration is 1mol/mL, the solution is fully mixed by magnetic stirring, and Li is finished when no solid precipitates2S6And (4) preparing.
b. Polysulfide shuttle experiment: the five-layer diaphragm prepared above and a polyolefin diaphragm are respectively clamped, and the left side is 10mL of Li with 1mol/mL2S6The right side is a colorless, transparent and pure DOL/DME solution. The shuttle effect of the polysulfides was compared after standing for 1 day, and the right-hand solution of the five-layer separator prepared using the present invention was found to have almost no change in color as shown in fig. 4, while the right-hand solution of the polyolefin separator had a large amount of polysulfide penetrated as shown in fig. 5, demonstrating the excellent inhibitory effect of the separator prepared according to the present invention on the polysulfides.
c. Assembling the lithium-sulfur battery: the lithium-sulfur battery is assembled into the button cell in a layer-by-layer stacking manner, wherein the first layer is a lithium sheet (with the thickness of 0.5 mm); the second layer is an aramid nanofiber/PDDA or polyolefin membrane; and the third layer is a C/S electrode, a plurality of drops of electrolyte are dripped, the assembly and compaction are carried out, namely the assembly of the lithium-sulfur battery is completed, and the electrochemical performance of the battery is tested. The tested performance includes cyclic voltammetry, cyclic stability measurement and rate performance.
The cycle performance of the lithium-sulfur battery using the ANF/PDDA diaphragm can still keep stable cycle above 10000 circles, while the traditional polyolefin diaphragm can only keep about 500 circles, which shows that the stability of the battery is obviously improved.
Claims (5)
1. A preparation method of a lithium-sulfur battery diaphragm based on multilayer aramid nanofibers is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: preparing an aramid nanofiber solution:
adding aramid fiber into a sealed dimethyl sulfoxide (DMSO) wire-mouth bottle, adding potassium hydroxide, and magnetically stirring at room temperature for reaction for 2 weeks until the aramid fiber is completely dissolved and the solution is dark red, thereby completing the preparation of the aramid nanofiber solution;
step two: preparing a multilayer aramid nanofiber membrane:
dropwise adding the aramid fiber nanofiber solution obtained in the step one onto a rectangular glass sheet, rotating the rectangular glass sheet at a speed of 1500r/min for 30s, simultaneously soaking the rectangular glass sheet into deionized water, standing for 1 day, continuously replacing the deionized water until dimethyl sulfoxide in the solution is completely removed, drying in an oven after the dimethyl sulfoxide in the solution is completely removed, soaking a diaphragm in 0.1 wt% of PDDA solution for 30s, washing the redundant PDDA solution on the surface with the deionized water after the diaphragm is taken out, drying in the oven, and sequentially repeating the operations of suspension coating, soaking and suspension coating to obtain a diaphragm with 5 layers.
2. The preparation method of the lithium-sulfur battery separator based on the multilayer aramid nanofibers, according to claim 1, is characterized in that: in the first step, the mass ratio of the aramid fiber, dimethyl sulfoxide and potassium hydroxide is 2: 98: 3.
3. the preparation method of the lithium-sulfur battery separator based on the multilayer aramid nanofibers, according to claim 1, is characterized in that: in the second step, every 1-5 mL of aramid nano-fiber solution is dripped on a rectangular glass sheet with the length multiplied by the width of 60-80 mm multiplied by 30-50 mm.
4. The preparation method of the lithium-sulfur battery separator based on the multilayer aramid nanofibers, according to claim 1, is characterized in that: in the second step, the continuous replacement means replacement every 3 to 5 hours.
5. The preparation method of the lithium-sulfur battery separator based on the multilayer aramid nanofibers, according to claim 1, is characterized in that: in the second step, the drying temperature is 40-70 ℃, and the drying time is 10-60 min.
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Cited By (2)
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| CN113422156A (en) * | 2021-07-27 | 2021-09-21 | 广东电网有限责任公司 | Modified diaphragm material, modified diaphragm and lithium-sulfur button cell |
| CN114573983A (en) * | 2022-03-16 | 2022-06-03 | 哈尔滨工业大学 | Preparation method of nano-diamond/aramid nanofiber multifunctional composite heat-conducting film |
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