CN115513605B - Lithium-sulfur battery diaphragm based on functional carbon material, and preparation method and application thereof - Google Patents
Lithium-sulfur battery diaphragm based on functional carbon material, and preparation method and application thereof Download PDFInfo
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- CN115513605B CN115513605B CN202211264677.7A CN202211264677A CN115513605B CN 115513605 B CN115513605 B CN 115513605B CN 202211264677 A CN202211264677 A CN 202211264677A CN 115513605 B CN115513605 B CN 115513605B
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- carbon material
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- sulfur battery
- diaphragm
- lithium sulfur
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 42
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000004743 Polypropylene Substances 0.000 claims abstract description 23
- 239000002033 PVDF binder Substances 0.000 claims abstract description 22
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229920001155 polypropylene Polymers 0.000 claims abstract description 22
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 22
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- -1 polypropylene Polymers 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 15
- 108010010803 Gelatin Proteins 0.000 claims description 13
- 229920000159 gelatin Polymers 0.000 claims description 13
- 239000008273 gelatin Substances 0.000 claims description 13
- 235000019322 gelatine Nutrition 0.000 claims description 13
- 235000011852 gelatine desserts Nutrition 0.000 claims description 13
- 229920000877 Melamine resin Polymers 0.000 claims description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 229920001021 polysulfide Polymers 0.000 abstract description 9
- 239000005077 polysulfide Substances 0.000 abstract description 9
- 150000008117 polysulfides Polymers 0.000 abstract description 9
- 125000005842 heteroatom Chemical group 0.000 abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000001351 cycling effect Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910018091 Li 2 S Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- DLGYNVMUCSTYDQ-UHFFFAOYSA-N azane;pyridine Chemical compound N.C1=CC=NC=C1 DLGYNVMUCSTYDQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Classifications
-
- 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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
-
- 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
-
- 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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
-
- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/491—Porosity
-
- 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 relates to a lithium sulfur battery diaphragm based on a functional carbon material, a preparation method and application thereof, wherein the lithium sulfur battery diaphragm is prepared by coating a functional coating consisting of a functional carbon material NGC, conductive carbon black AB and polyvinylidene fluoride PVDF on a polypropylene diaphragm. According to the invention, the functional coating containing the heteroatom doped carbon material and the conductive carbon black is coated on the surface of the diaphragm to form the functional diaphragm for the lithium sulfur battery, and the shuttle of polysulfide is inhibited by the functional diaphragm, so that the cycle stability of the lithium sulfur battery is improved.
Description
Technical Field
The invention belongs to the field of lithium-sulfur batteries, and particularly relates to a lithium-sulfur battery diaphragm based on a functional carbon material, and a preparation method and application thereof.
Background
With the widespread use of power automobiles and large energy storage systems, the market places considerable demands on the performance of chemical power sources, particularly on the energy density requirements of batteries. Based on S 8 +16Li=8Li 2 S, rechargeable lithium sulfur batteries are receiving attention due to their high energy density. In addition, the advantages of low toxicity, abundant reserves, low cost and the like of the elemental sulfur lead the lithium sulfur battery to have wide commercial application prospect. However, despite these significant advantages, the development of lithium sulfur batteries is hampered by the following problems: (1) Elemental sulfur and discharge product Li 2 S 2 /Li 2 The electrical insulation of S requires the addition of a certain amount of conductive agent to the positive electrode material, resulting in a practical batteryThe energy density decreases; (2) Polysulfide can be dissolved into electrolyte during discharge, so that rapid capacity attenuation, low coulomb efficiency and corrosion of the surface of the cathode are caused; (3) Elemental sulfur and Li during charge and discharge 2 S 2 /Li 2 The difference in density of S causes expansion and contraction of the positive electrode, resulting in destruction of the electrode structure.
In order to solve the above problems, researchers have explored different strategies such as positive electrode materials of different structures, negative electrode surface protection and design of novel electrolyte systems, thereby effectively improving the electrochemical performance of lithium-sulfur batteries. In addition, the functional coating is constructed on the surface of the diaphragm, so that the diffusion of polysulfide can be effectively inhibited. Among other things, commonly used functional coatings include porous carbon-based materials that are capable of physically blocking polysulfides and improving the utilization of active substances. However, van der Waals forces between nonpolar carbon materials and polar polysulfides are weak, resulting in rapid capacity decay of the battery.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a lithium sulfur battery diaphragm based on a functional carbon material, a preparation method and application thereof, wherein a layer of functional coating containing heteroatom doped carbon material and conductive carbon black is coated on the surface of the diaphragm to form the functional diaphragm for the lithium sulfur battery, and shuttle of polysulfide is inhibited by the functional diaphragm, so that the cycling stability of the lithium sulfur battery is improved.
In order to achieve the aim of the invention, the invention adopts the following technical scheme: a lithium sulfur battery diaphragm based on a functional carbon material is obtained by coating a functional coating consisting of a functional carbon material NGC, conductive carbon black AB and polyvinylidene fluoride PVDF on a polypropylene diaphragm.
In a preferred embodiment of the invention, the mass ratio of the functional carbon material NGC, the conductive carbon black AB and the polyvinylidene fluoride PVDF is 1-3:1-3:0.5-2, and more preferably 2:2:1.
In a preferred embodiment of the present invention, the functional carbon material NGC is prepared from melamine and gelatin by heat treatment.
In a preferred embodiment of the present invention, the preparation method of the functional carbon material NGC includes the following steps:
(1) Ball milling melamine and gelatin respectively, and mixing uniformly;
(2) And (3) performing heat treatment on the mixture obtained in the step (1).
In a preferred embodiment of the present invention, the mass ratio of melamine to gelatin is 5-20:0.5-2, more preferably 10:1.
In a preferred embodiment of the invention, the heat treatment is: and (3) heating to 300-500 ℃ at a heating rate of 1-3 ℃/min under nitrogen atmosphere and preserving heat for 0.5-2 hours, and then heating to 700-900 ℃ at a heating rate of 4-6 ℃/min and preserving heat for 0.5-2 hours to finally obtain the carbon material NGC.
The invention also provides a preparation method of the lithium sulfur battery diaphragm based on the functional carbon material, which comprises the following steps: and mixing the functional carbon material NGC, the conductive carbon black AB and the polyvinylidene fluoride PVDF, uniformly stirring, uniformly coating on the PP diaphragm, and drying to obtain the lithium-sulfur battery diaphragm based on the functional carbon material.
In a preferred embodiment of the invention, the mass ratio of the functional carbon material NGC, the conductive carbon black AB and the polyvinylidene fluoride PVDF is 1-3:1-3:0.5-2, and more preferably 2:2:1.
In a preferred embodiment of the present invention, the drying temperature is 50 to 70 ℃.
The invention also protects application of the lithium sulfur battery diaphragm in preparing a lithium sulfur battery.
Compared with the prior art, the invention has the following beneficial effects:
the invention converts melamine into graphitized carbon nitride nano-sheets at high temperature, and takes the graphitized carbon nitride nano-sheets as a soft template, so that the carbon material grows into a sheet-shaped structure on the template. Further raising the temperature, the graphitized carbon nitride is decomposed into nitrogen-containing gas, and the nitrogen-containing gas is doped in situ in the carbon material, so that the carbon material with high heteroatom content and high conductivity is finally prepared. And mixing the prepared carbon material with conductive carbon black, and coating the mixture on the surface of a commercial diaphragm to finally obtain the functional diaphragm.
The layered porous carbon material on the functional membrane can physically block the diffusion of polysulfide, and abundant heteroatoms contained in the layered porous carbon material can effectively fix polysulfide. In addition, the pyridine nitrogen contained in the carbon material can provide lone pair electrons, so that the redox conversion of sulfur species is accelerated. Thanks to the conductive network of carbon material and carbon black on the functional separator, the adsorbed polysulfide will get the lost electrons to be reused, and the utilization efficiency of the active substance is increased. Thus, the cycle stability of the battery employing the functional separator is significantly improved.
Drawings
The following is further described with reference to the accompanying drawings:
FIG. 1 is an SEM image of the surface of a GC/PP functional separator according to example 1 of the present invention;
FIG. 2 is a graph of cycling performance at 1C for lithium sulfur batteries employing different separators;
FIG. 3 is an SEM image of the surface of an NGC/PP functional separator according to example 2 of the invention;
fig. 4 is a graph of the cycling performance of a lithium sulfur battery employing different separators at 1C (increasing the cycling performance of the NGC/PP functional separator obtained in example 2).
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto, and any modification or variation in form of the present invention should be considered as falling within the scope of the present invention.
Example 1
And (3) carrying out heat preservation on the gelatin of 0.5 g to 400 ℃ at a heating rate of 2 ℃/min for 1 hour under a nitrogen atmosphere, and then carrying out heat preservation on the gelatin for 1 hour at a heating rate of 5 ℃/min to 800 ℃ to finally obtain the gelatin carbon material (GC). 0.4g of GC,0.4 g of conductive carbon black (AB) and 0.2. 0.2 g of polyvinylidene fluoride (PVDF) are magnetically stirred, then uniformly coated on a polypropylene (PP) diaphragm, and the GC/PP functional diaphragm is obtained after drying.
The surface morphology of the GC/PP functional separator was observed using a scanning electron microscope to give fig. 1. As can be seen from fig. 1, the surface of the separator is uniformly distributed with the block carbon material and the granular conductive carbon black.
The obtained functional diaphragm is cut into 17 mm wafers, a CR 2025 button cell is assembled in a glove box by utilizing a sulfur anode, a lithium cathode and a lithium sulfur cell electrolyte, and is subjected to a cycle test at 1C on a constant current charge-discharge instrument, and lithium sulfur cells with different diaphragms are also subjected to the cycle test under the same conditions, wherein the PP diaphragm refers to a polypropylene diaphragm, the AB/PP diaphragm refers to an acetylene black modified polypropylene diaphragm, and the GC diaphragm is a Gelatin Carbon (GC) modified polypropylene diaphragm which does not adopt the soft template of the invention. The results are shown in FIG. 2. As can be seen from fig. 2, the functional separator (GC/PP separator) prepared using the carbon material prepared with gelatin of example 1 exhibited the highest discharge capacity and capacity retention rate.
Example 2
5 g melamine and 0.5 g gelatin are ball milled uniformly. Then placing the obtained mixture in a crucible, and preserving the temperature for 1 hour at the temperature rising speed of 2 ℃/min to 400 ℃ under the nitrogen atmosphere, and then preserving the temperature for 1 hour at the temperature rising speed of 5 ℃/min to 800 ℃ to finally obtain the nitrogen-enriched gelatin carbon material (i.e. nitrogen-rich gelatin carbon, abbreviated as NGC). 0.4g of NGC,0.4 g of conductive carbon black (AB) and 0.2. 0.2 g of polyvinylidene fluoride (PVDF) are magnetically stirred, then uniformly coated on a polypropylene (PP) membrane, and dried to obtain the NGC/PP functional membrane.
The surface morphology of the NGC/PP functional membrane was observed by a scanning electron microscope to obtain FIG. 3. As can be seen from fig. 3, the surface of the separator is uniformly distributed with the sheet carbon material and the granular conductive carbon black.
The obtained functional separator was cut into 17 mm discs, CR 2025 button cell was assembled in a glove box using a sulfur positive electrode, a lithium negative electrode and a lithium sulfur battery electrolyte, and was subjected to a cycle test at 1C on a constant current charge-discharge meter, and lithium sulfur batteries of different separators were also subjected to a cycle test under the same conditions, the results of which are shown in fig. 4. As can be seen from fig. 4, the functional separator (NGC/PP separator) prepared by using the carbon material of the soft template of the present application shows the highest discharge capacity and capacity retention.
Those skilled in the art will recognize that a wide variety of modifications, alterations, and combinations can be made with respect to the above described embodiments without departing from the scope of the invention, and that such modifications, alterations, and combinations are to be viewed as being within the ambit of the inventive concept.
Claims (6)
1. A lithium sulfur battery diaphragm based on a functional carbon material is characterized in that a functional coating consisting of a functional carbon material NGC, conductive carbon black AB and polyvinylidene fluoride PVDF is coated on a polypropylene diaphragm to obtain the diaphragm; the mass ratio of the functional carbon material NGC, the conductive carbon black AB and the polyvinylidene fluoride PVDF is 1-3:1-3:0.5-2; the preparation method of the functional carbon material NGC comprises the following steps:
(1) Ball milling melamine and gelatin respectively, and mixing uniformly;
(2) Carrying out heat treatment on the mixture obtained in the step (1);
the mass ratio of the melamine to the gelatin is 10:1.
2. The lithium sulfur battery separator according to claim 1, wherein the mass ratio of the functional carbon material NGC, the conductive carbon black AB and the polyvinylidene fluoride PVDF is 2:2:1.
3. The lithium sulfur battery separator according to claim 1, wherein the heat treatment is: heating to 300-500 ℃ at a heating rate of 1-3 ℃/min under nitrogen atmosphere and preserving heat for 0.5-2 hours, then heating to 700-800 ℃ at a heating rate of 4-6 ℃/min and preserving heat for 0.5-2 hours, and finally obtaining the carbon material NGC.
4. A method for producing a lithium sulfur battery separator according to any one of claims 1 to 3, comprising the steps of: and mixing the functional carbon material NGC, the conductive carbon black AB and the polyvinylidene fluoride PVDF, uniformly stirring, uniformly coating on the PP diaphragm, and drying to obtain the lithium-sulfur battery diaphragm based on the functional carbon material.
5. The process according to claim 4, wherein the drying temperature is 50 to 70 ℃.
6. Use of a lithium sulfur battery separator according to any one of claims 1-3 or a lithium sulfur battery separator prepared by a preparation method according to any one of claims 4-5 in the preparation of a lithium sulfur battery.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211264677.7A CN115513605B (en) | 2022-10-17 | 2022-10-17 | Lithium-sulfur battery diaphragm based on functional carbon material, and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211264677.7A CN115513605B (en) | 2022-10-17 | 2022-10-17 | Lithium-sulfur battery diaphragm based on functional carbon material, and preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN115513605A CN115513605A (en) | 2022-12-23 |
| CN115513605B true CN115513605B (en) | 2024-03-08 |
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| CN115513605A (en) | 2022-12-23 |
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