CN112271402A - Method for preparing carbon-point modified lithium-sulfur battery diaphragm by taking cellulose acetate as carbon source - Google Patents
Method for preparing carbon-point modified lithium-sulfur battery diaphragm by taking cellulose acetate as carbon source Download PDFInfo
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Abstract
The invention relates to a method for preparing a lithium-sulfur battery diaphragm by using cellulose acetate as a carbon source and modifying a carbon point, belonging to the technical field of battery diaphragm materials. The method comprises the following steps: the method comprises the following steps: preparing carbon dots by taking cellulose acetate as a carbon source; step two: preparing a carbon point modified diaphragm for a lithium-sulfur battery, namely adding conductive carbon black and a binder into the carbon points obtained in the step one, preparing a mixture according to 50-90wt% of the carbon points, 5-40wt% of the conductive carbon black and 5-40wt% of the binder, and adding a dispersing agent into the mixture to prepare slurry; the slurry was coated onto a polypropylene separator with a coating thickness of 100-300 μm, and dried under vacuum at 50 ℃ to obtain a carbon-modified separator for a lithium-sulfur battery. The carbon dots can be doped with N/S to further improve the performance of the lithium sulfur battery. Meanwhile, a way is provided for the use of cellulose acetate and the recycling of cigarette butts.
Description
Technical Field
The invention belongs to the technical field of battery diaphragm materials, and particularly relates to a method for preparing a carbon-point modified lithium-sulfur battery diaphragm by taking cellulose acetate as a carbon source.
Background
As a new generation of lithium ion battery with the most commercial application potential, the lithium sulfur battery has the characteristics of high specific capacity, rich resources, environmental friendliness and the like. However, the lithium-sulfur battery has poor conductivity of sulfur and its discharge product (lithium sulfide), serious volume change in electrochemical process, and problems of dissolution of long-chain polysulfide in organic electrolyte and shuttling between positive and negative electrodes during charging and discharging process, which seriously affect the coulombic efficiency and cycle life. Research shows that the electrochemical performance of the lithium-sulfur battery can be remarkably improved by coating the material with the adsorption effect on the polysulfide compound on the surface of the commercial polypropylene diaphragm. For example, by using the polar-polar interaction between graphene oxide, metal oxygen/sulfur/nitrogen/carbide, and the like and polysulfide, the polysulfide can be firmly bound. However, these polar materials are expensive or complicated in preparation process, and can be obtained by high-temperature oxidation, vulcanization or nitrogen/carbonization, which is not suitable for large-scale application.
Disclosure of Invention
The invention aims to solve the problems that: the invention provides a method for modifying a lithium-sulfur battery diaphragm by using carbon points, which is prepared by using cellulose acetate as a carbon source, aiming at the problems of high raw material cost, complex preparation process and the like existing in the commonly adopted polar graphene oxide, metal oxygen/sulfur/nitrogen/carbide and the like coated polypropylene diaphragm during the modification of the lithium-sulfur battery diaphragm.
The technical scheme of the invention is as follows: the method for preparing the carbon point modified lithium-sulfur battery diaphragm by taking the cellulose acetate as the carbon source is characterized by comprising the following steps of:
the method comprises the following steps: carbon dots prepared by taking cellulose acetate as carbon source
Placing cellulose acetate in a solvent, and magnetically stirring for 30 minutes to completely disperse the cellulose acetate in the solvent; transferring the mixture to a hydrothermal reaction kettle for hydrothermal reaction; washing and drying the reacted substances to obtain carbon dots;
step two: preparation of carbon-point-modified diaphragm for lithium-sulfur battery
Adding conductive carbon black and a binder into the carbon dots obtained in the step one, preparing a mixture according to 50-90wt% of the carbon dots, 5-40wt% of the conductive carbon black and 5-40wt% of the binder, and adding a dispersant into the mixture to prepare slurry; the slurry was coated onto a polypropylene separator with a coating thickness of 100-300 μm, and dried under vacuum at 50 ℃ to obtain a carbon-modified separator for a lithium-sulfur battery.
Further, one or two of urea or cysteine is added into the mixture of the cellulose acetate and the solvent in the step one, and the N/S doped carbon point or the N, S co-doped carbon point is synthesized.
Further, the cellulose acetate in the first step comprises cellulose acetate sheets, cellulose acetate fibers or recycled cigarette end filters synthesized by cellulose acetate fibers.
Further, the solvent in the step one is distilled water or absolute ethyl alcohol;
further, the temperature of the hydrothermal reaction in the first step is 120-.
The invention has the beneficial effects that:
1. the carbon dots prepared by the method have small size, the diameter is about 50nm, and active groups such as hydroxyl, amino and the like are arranged on the surface of the carbon dots, so that a large number of polar sites are provided for the adsorption of polysulfide;
2. after the carbon point modified diaphragm is used, the initial discharge specific capacity of the lithium-sulfur battery under 1C reaches 1151mAh g-1After 600 cycles, 652mAh g is still kept-1Specific discharge capacity of (2). Compared with the diaphragm without carbon point modification (the initial capacity of 1C is only 116mAh g-1) After 20 cycles, the capacity decayed sharply to 100mAh g-1The performance of the lithium-sulfur battery is greatly improved;
3. according to the invention, the N/S doped carbon dots with stronger polarity are obtained by adding the nitrogen source or the sulfur source in the preparation process, so that the adsorption effect between the carbon dots and the polysulfide compound can be further enhanced; after the N-doped carbon point modified diaphragm, the initial discharge specific capacity of the lithium-sulfur battery under 1C reaches 1121mAh g-1After 600 times of circulation, 703mAh g is still kept-1Specific discharge capacity of (a); after the S-doped carbon point modified diaphragm is adopted, the initial discharge specific capacity of the lithium-sulfur battery under 1C reaches 1086mAh g-1After 600 cycles, 693mAh g remained-1Specific discharge capacity of (a); n, S the initial discharge specific capacity of the lithium-sulfur battery under 1C reaches 1214mAh g-1756mAh g remained after 600 cycles-1Specific discharge capacity of (2).
4. The invention also provides a way for the use of cellulose acetate and the recycling of cigarette butts.
Detailed Description
Comparative example:
and (3) assembling the button cell by taking the polypropylene diaphragm as the diaphragm of the lithium-sulfur cell, the metal lithium sheet as the negative electrode and the sulfur as the positive electrode. Wherein the anode material is prepared by mixing sublimed sulfur, conductive carbon black and polyvinylidene fluoride according to the weight ratio of 7: 2: 1, and then, a slurry prepared by adding methyl pyrrolidone was applied to an aluminum foil in a thickness of 150 μm. Through testing, the initial discharge specific capacity of the lithium-sulfur battery under 1C is 116mAh g-1After 20 cycles, the capacity decayed sharply to 100mAh g-1The following.
Example 1:
the method for preparing the carbon point modified lithium-sulfur battery diaphragm by taking the cellulose acetate as the carbon source comprises the following steps:
the method comprises the following steps: preparation of carbon dots by using cellulose acetate sheet as carbon source
Placing 500mg cellulose acetate tablets in 30mL absolute ethyl alcohol, and magnetically stirring for 30 minutes to completely disperse the cellulose acetate tablets in the absolute ethyl alcohol; transferring the mixture to a hydrothermal reaction kettle to react for 15 hours at the temperature of 160 ℃; and washing and drying the reacted substance to obtain carbon dots.
Step two: preparation of carbon-point-modified diaphragm for lithium-sulfur battery
Adding conductive carbon black and a binder into the carbon dots obtained in the step one, preparing a mixture by 60 wt% of the carbon dots, 5-40wt% of the conductive carbon black and 5-40wt% of a polyvinylidene fluoride binder, and adding N-methyl pyrrolidone into the mixture to prepare slurry; the slurry was coated on a polypropylene separator to a thickness of 300 μm, and vacuum-dried at 50 ℃ to obtain a carbon-dot modified separator for a lithium-sulfur battery.
Step three: lithium sulfur cell button cell assembly and electrochemical performance testing
Using the carbon point modified diaphragm in the step two as a diaphragm of a lithium-sulfur battery and a metal lithium sheetAnd the button cell is assembled by taking the sulfur as a negative electrode and taking the sulfur as a positive electrode, wherein the positive electrode material is prepared by mixing sublimed sulfur, conductive carbon black and polyvinylidene fluoride according to the weight ratio of 7: 2: 1, and then, a slurry prepared by adding methyl pyrrolidone was applied to an aluminum foil in a thickness of 150 μm. During the assembly of the button cell, the side coated with carbon dots and conductive carbon black faces the positive side. Tests prove that the initial discharge specific capacity of the lithium-sulfur battery under 1C reaches 887mAh g-1548mAh g is still kept after 300 times of circulation-1Specific discharge capacity of (2).
Example 2
The method for preparing the carbon point modified lithium-sulfur battery diaphragm by taking the cellulose acetate as the carbon source comprises the following steps:
the method comprises the following steps: preparation of carbon dots by using cellulose acetate fibers as carbon source
500mg of cellulose acetate fiber is put into 30mL of distilled water and is stirred for 30 minutes by magnetic force to be completely dispersed in the solvent; transferring the mixture to a hydrothermal reaction kettle to react for 12 hours at the temperature of 180 ℃; washing and drying the reacted substances to obtain carbon dots;
step two: preparation of carbon-point-modified diaphragm for lithium-sulfur battery
Adding conductive carbon black and a binder into the carbon dots obtained in the step one, preparing a mixture by 70 wt% of the carbon dots, 5-40wt% of the conductive carbon black and 5-40wt% of a polyvinylidene fluoride binder, and adding N-methyl pyrrolidone into the mixture to prepare slurry; the slurry was coated on a polypropylene separator to a thickness of 250 μm, and vacuum-dried at 50 ℃ to obtain a carbon-site-modified separator for a lithium-sulfur battery.
Step three: lithium sulfur cell button cell assembly and electrochemical performance testing
And taking the carbon dot modified diaphragm in the step two as a lithium-sulfur battery diaphragm, taking a metal lithium sheet as a negative electrode, and taking sulfur as a positive electrode to assemble the button battery, wherein the positive electrode material is prepared by mixing sublimed sulfur, conductive carbon black and polyvinylidene fluoride according to the weight ratio of 7: 2: 1, and then, a slurry prepared by adding methyl pyrrolidone was applied to an aluminum foil in a thickness of 150 μm. During the assembly of the button cell, the side coated with carbon dots and conductive carbon black faces the positive side. By testing, the lithiumThe initial discharge specific capacity of the sulfur battery under 1C reaches 935mAh g-1After 300 cycles, 652mAh g is still kept-1Specific discharge capacity of (2).
Example 3
The method for preparing the carbon point modified lithium-sulfur battery diaphragm by taking the cellulose acetate as the carbon source comprises the following steps:
the method comprises the following steps: carbon dots prepared by using cigarette end filter tip composed of cellulose acetate fiber as carbon source
Repeatedly soaking and cleaning the cigarette end filter tip without the coating paper by distilled water, and then drying for later use. Putting 500mg of the cigarette end filter tip into 30mL of distilled water, and magnetically stirring for 30 minutes to completely disperse the cigarette end filter tip into the solvent; transferring the mixture to a hydrothermal reaction kettle to react for 10 hours at the temperature of 200 ℃; and washing and drying the reacted substance to obtain carbon dots.
Step two: preparation of carbon-point-modified diaphragm for lithium-sulfur battery
Adding conductive carbon black and a binder into the carbon dots obtained in the step one, preparing a mixture by 80 wt% of the carbon dots, 5-40wt% of the conductive carbon black and 5-40wt% of a polyvinylidene fluoride binder, and adding N-methyl pyrrolidone into the mixture to prepare slurry; and coating the slurry on a polypropylene diaphragm to a coating thickness of 200 mu m, and performing vacuum drying at 50 ℃ to obtain the carbon dot modified diaphragm for the lithium-sulfur battery.
Step three: lithium sulfur cell button cell assembly and electrochemical performance testing
And taking the carbon dot modified diaphragm in the step two as a lithium-sulfur battery diaphragm, taking a metal lithium sheet as a negative electrode, and taking sulfur as a positive electrode to assemble the button battery, wherein the positive electrode material is prepared by mixing sublimed sulfur, conductive carbon black and polyvinylidene fluoride according to the weight ratio of 7: 2: 1, and then, a slurry prepared by adding methyl pyrrolidone was applied to an aluminum foil in a thickness of 150 μm. During the assembly of the button cell, the side coated with carbon dots and conductive carbon black faces the positive side. Tests prove that the initial discharge specific capacity of the lithium-sulfur battery under 1C reaches 1151mAh g-1After 600 cycles, 652mAh g is still kept-1Specific discharge capacity of (2).
Example 4
The method for preparing the carbon point modified lithium-sulfur battery diaphragm by taking the cellulose acetate as the carbon source comprises the following steps:
the method comprises the following steps: preparation of N-doped carbon dots by using cigarette end filter tip composed of cellulose acetate fiber as carbon source and urea as nitrogen source
Repeatedly soaking and cleaning the cigarette end filter tip without the coating paper by distilled water, and then drying for later use. Putting 500mg of cigarette end filter tip into 30mL of distilled water, adding 100mg of urea into the distilled water, and magnetically stirring the mixture for 30 minutes to completely disperse the mixture in the solvent; transferring the mixture to a hydrothermal reaction kettle to react for 8 hours at the temperature of 220 ℃; and washing and drying the reacted substance to obtain carbon dots.
Step two: preparation of N-doped carbon point modified diaphragm for lithium-sulfur battery
Adding conductive carbon black and a binder into the carbon dots obtained in the step one, preparing a mixture by 90wt% of N-doped carbon dots, 5-40wt% of conductive carbon black and 5-40wt% of polyvinylidene fluoride binder, and adding N-methyl pyrrolidone into the mixture to prepare slurry; the slurry was coated on a polypropylene separator to a coating thickness of 150 μm, and vacuum-dried at 50 ℃ to obtain a carbon dot-modified separator for a lithium-sulfur battery.
Step three: lithium sulfur cell button cell assembly and electrochemical performance testing
And taking the carbon dot modified diaphragm in the step two as a lithium-sulfur battery diaphragm, taking a metal lithium sheet as a negative electrode, and taking sulfur as a positive electrode to assemble the button battery, wherein the positive electrode material is prepared by mixing sublimed sulfur, conductive carbon black and polyvinylidene fluoride according to the weight ratio of 7: 2: 1, and then, a slurry prepared by adding methyl pyrrolidone was applied to an aluminum foil in a thickness of 150 μm. During the assembly of the button cell, the side coated with carbon dots and conductive carbon black faces the positive side. Tests prove that the initial specific discharge capacity of the lithium-sulfur battery under 1C reaches 1121mAh g-1After 600 times of circulation, 703mAh g is still kept-1Specific discharge capacity of (2).
Example 5
The method for preparing the carbon point modified lithium-sulfur battery diaphragm by taking the cellulose acetate as the carbon source comprises the following steps:
the method comprises the following steps: preparation of S-doped carbon dots by using cigarette butt filter tip composed of cellulose acetate fiber as carbon source and cysteine as sulfur source
Repeatedly soaking and cleaning the cigarette end filter tip without the coating paper by distilled water, and then drying for later use. Putting 500mg of cigarette end filter tip into 30mL of distilled water, adding 100mg of cysteine into the distilled water, and magnetically stirring the mixture for 30 minutes to completely disperse the mixture in the solvent; transferring the mixture to a hydrothermal reaction kettle to react for 8 hours at the temperature of 220 ℃; and washing and drying the reacted substance to obtain carbon dots.
Step two: preparation of S-doped carbon point modified diaphragm for lithium-sulfur battery
Adding conductive carbon black and a binder into the carbon dots obtained in the step one, preparing a mixture by 90wt% of N-doped carbon dots, 5-40wt% of conductive carbon black and 5-40wt% of polyvinylidene fluoride binder, and adding N-methyl pyrrolidone into the mixture to prepare slurry; the slurry was coated on a polypropylene separator to a coating thickness of 100 μm, and vacuum-dried at 50 ℃ to obtain a carbon dot-modified separator for a lithium-sulfur battery.
Step three: lithium sulfur cell button cell assembly and electrochemical performance testing
And taking the carbon dot modified diaphragm in the step two as a lithium-sulfur battery diaphragm, taking a metal lithium sheet as a negative electrode, and taking sulfur as a positive electrode to assemble the button battery, wherein the positive electrode material is prepared by mixing sublimed sulfur, conductive carbon black and polyvinylidene fluoride according to the weight ratio of 7: 2: 1, and then, a slurry prepared by adding methyl pyrrolidone was applied to an aluminum foil in a thickness of 150 μm. During the assembly of the button cell, the side coated with carbon dots and conductive carbon black faces the positive side. Tests prove that the initial discharge specific capacity of the lithium-sulfur battery under 1C reaches 1086mAhg-1After 600 cycles, 693mAhg of the product is still retained-1Specific discharge capacity of (2).
Example 6
The method for preparing the carbon point modified lithium-sulfur battery diaphragm by taking the cellulose acetate as the carbon source comprises the following steps:
the method comprises the following steps: the N, S co-doped carbon dots are prepared by taking a cigarette butt filter tip consisting of cellulose acetate fibers as a carbon source, urea as a nitrogen source and cysteine as a sulfur source.
Repeatedly soaking and cleaning the cigarette end filter tip without the coating paper by distilled water, and then drying for later use. Putting 500mg of cigarette end filter tip into 30mL of distilled water, adding 100mg of urea and 40mg of cysteine into the distilled water, and magnetically stirring the mixture for 30 minutes to completely disperse the mixture into the distilled water; transferring the mixture to a hydrothermal reaction kettle to react for 8 hours at the temperature of 220 ℃; and washing and drying the reacted substance to obtain carbon dots.
Step two: n, S preparation of co-doped carbon point modified diaphragm for lithium-sulfur battery
Adding conductive carbon black and a binder into the carbon dots obtained in the step one, preparing a mixture by co-doping the carbon dots with N, S wt%, 5-40wt% of conductive carbon black and 5-40wt% of polyvinylidene fluoride binder, and adding N-methyl pyrrolidone into the mixture to prepare slurry; the slurry was coated on a polypropylene separator to a coating thickness of 100 μm, and vacuum-dried at 50 ℃ to obtain a carbon dot-modified separator for a lithium-sulfur battery.
Step three: lithium sulfur cell button cell assembly and electrochemical performance testing
And taking the carbon dot modified diaphragm in the step two as a lithium-sulfur battery diaphragm, taking a metal lithium sheet as a negative electrode, and taking sulfur as a positive electrode to assemble the button battery, wherein the positive electrode material is prepared by mixing sublimed sulfur, conductive carbon black and polyvinylidene fluoride according to the weight ratio of 7: 2: 1, and then, a slurry prepared by adding methyl pyrrolidone was applied to an aluminum foil in a thickness of 150 μm. During the assembly of the button cell, the side coated with carbon dots and conductive carbon black faces the positive side. Tests prove that the initial specific discharge capacity of the lithium-sulfur battery under 1C reaches 1214mAh g-1756mAh g remained after 600 cycles-1Specific discharge capacity of (2).
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (5)
1. The method for preparing the carbon point modified lithium-sulfur battery diaphragm by taking the cellulose acetate as the carbon source is characterized by comprising the following steps of:
the method comprises the following steps: carbon dots prepared by taking cellulose acetate as carbon source
Placing cellulose acetate in a solvent, and magnetically stirring for 30 minutes to completely disperse the cellulose acetate in the solvent; transferring the mixture to a hydrothermal reaction kettle for hydrothermal reaction; washing and drying the reacted substances to obtain carbon dots;
step two: preparation of carbon-point-modified diaphragm for lithium-sulfur battery
Adding conductive carbon black and a binder into the carbon dots obtained in the step one, preparing a mixture according to 50-90wt% of the carbon dots, 5-40wt% of the conductive carbon black and 5-40wt% of the binder, and adding a dispersant into the mixture to prepare slurry; the slurry was coated onto a polypropylene separator with a coating thickness of 100-300 μm, and dried under vacuum at 50 ℃ to obtain a carbon-modified separator for a lithium-sulfur battery.
2. The method for preparing the carbon point modified lithium-sulfur battery separator by using the cellulose acetate as the carbon source according to claim 1, wherein one or two of urea and cysteine are added into the mixture of the cellulose acetate and the solvent in the step one to synthesize the N/S doped carbon point or the N, S co-doped carbon point.
3. The method for preparing the carbon-point modified lithium sulfur battery separator using cellulose acetate as the carbon source according to claim 1, wherein the cellulose acetate in the first step comprises a cellulose acetate sheet, a cellulose acetate fiber or a recycled cigarette end filter synthesized from cellulose acetate fibers.
4. The method for preparing the carbon-point modified lithium-sulfur battery separator by using the cellulose acetate as the carbon source according to claim 1, wherein the solvent in the first step is distilled water or absolute ethyl alcohol.
5. The method for preparing the carbon-point modified lithium-sulfur battery separator by using the cellulose acetate as the carbon source as claimed in claim 1, wherein the temperature of the hydrothermal reaction in the first step is 120-200 ℃, and the reaction time is 8-15 hours.
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