CN113964291A - High-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate and preparation method thereof, and lithium fluorocarbon battery - Google Patents
High-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate and preparation method thereof, and lithium fluorocarbon battery Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000000956 alloy Substances 0.000 title claims abstract description 75
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 75
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 74
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 74
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 150000002641 lithium Chemical class 0.000 title claims abstract description 35
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 22
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 36
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011888 foil Substances 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 19
- 238000000576 coating method Methods 0.000 claims abstract description 19
- 239000003792 electrolyte Substances 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 17
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011230 binding agent Substances 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 239000011267 electrode slurry Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- YBDACTXVEXNYOU-UHFFFAOYSA-N C(F)(F)(F)F.[Li] Chemical compound C(F)(F)(F)F.[Li] YBDACTXVEXNYOU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 26
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 15
- 229910017052 cobalt Inorganic materials 0.000 claims description 15
- 239000010941 cobalt Substances 0.000 claims description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 15
- 229910052738 indium Inorganic materials 0.000 claims description 15
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 15
- 229910052742 iron Inorganic materials 0.000 claims description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 14
- 229910052759 nickel Inorganic materials 0.000 claims description 14
- 229910052725 zinc Inorganic materials 0.000 claims description 14
- 239000011701 zinc Substances 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- -1 carbon nanotube modified lithium carbon fluoride Chemical class 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229920002125 Sokalan® Polymers 0.000 claims description 10
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 10
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 239000004584 polyacrylic acid Substances 0.000 claims description 8
- 239000002033 PVDF binder Substances 0.000 claims description 7
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical group N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 229910000337 indium(III) sulfate Inorganic materials 0.000 claims description 5
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004246 zinc acetate Substances 0.000 claims description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 5
- 229960001763 zinc sulfate Drugs 0.000 claims description 5
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 229910021446 cobalt carbonate Inorganic materials 0.000 claims description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 4
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims description 4
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 4
- 229940045803 cuprous chloride Drugs 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 229960002413 ferric citrate Drugs 0.000 claims description 3
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims description 3
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 3
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- 229940010514 ammonium ferrous sulfate Drugs 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 229960002089 ferrous chloride Drugs 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 2
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical group [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 claims description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 2
- ZEYKLMDPUOVUCR-UHFFFAOYSA-N 2-chloro-5-(trifluoromethyl)benzenesulfonyl chloride Chemical compound FC(F)(F)C1=CC=C(Cl)C(S(Cl)(=O)=O)=C1 ZEYKLMDPUOVUCR-UHFFFAOYSA-N 0.000 claims 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000006256 anode slurry Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- UEUDBBQFZIMOQJ-UHFFFAOYSA-K ferric ammonium oxalate Chemical compound [NH4+].[NH4+].[NH4+].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O UEUDBBQFZIMOQJ-UHFFFAOYSA-K 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical group [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002815 nickel Chemical group 0.000 description 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Images
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate and a preparation method thereof, wherein the preparation method comprises the following steps: step 1, preparing a high-entropy alloy/carbon nanotube composite material; step 2, weighing 70-90% of carbon fluoride, 5-20% of high-entropy alloy/carbon nanotube composite material and 5-10% of binder according to mass percent, grinding and mixing uniformly, then adding a solvent, and stirring uniformly to obtain a positive electrode slurry with fluidity; and 3, uniformly coating the positive electrode slurry on an aluminum foil or a carbon-coated aluminum foil by using a film coater, and drying and removing the solvent in vacuum to obtain the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive electrode sheet. The invention also provides a lithium fluorocarbon battery, which comprises electrolyte, a diaphragm, a negative plate and the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate. The positive plate prepared by the invention can improve the conductivity and rate capability of the lithium-carbon fluoride battery and improve the specific energy and storage performance of the battery.
Description
Technical Field
The invention relates to a lithium fluorocarbon battery, in particular to a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate, a preparation method thereof and a lithium fluorocarbon battery.
Background
Currently, lithium ion batteries are widely used in portable electronic products and electric vehicles, but there is still a need for battery systems that are cheaper, more advanced, higher in energy and power density, and better in safety. Among them, carbon fluoride (CFx) is one of the highest positive electrode materials of primary lithium batteries. Therefore, the Li/CFx primary battery is significantly superior to other competing primary lithium batteries, and has an ultra-long shelf life, a wide operating temperature range, and a flat discharge voltage. However, the rate performance of Li/CFx cells is poor because the electron conductivity of CFx decreases with increasing fluorine content. These inherent disadvantages severely hamper their use in high power devices.
Therefore, based on these problems, it is important to provide a positive electrode sheet capable of improving the specific energy and storage performance of a lithium carbon fluoride battery and improving the conductivity and rate performance of the positive electrode.
High Entropy Alloys (HEA) are an emerging material comprising five or more metal elements that are uniformly mixed in crystalline solid solution and stabilized by high entropy of mixing. Due to its superior physicochemical properties, including broad selection of elements, high corrosion resistance, high thermal and chemical stability, enhanced mechanical strength, recently received great attention in energy and catalytic applications, due to the synergistic catalytic reaction of elements, catalytic activity is enhanced.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate capable of improving the conductivity and rate performance of a positive electrode, a preparation method thereof and a lithium fluorocarbon battery with higher specific energy and storage performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate comprises the following steps:
step 1, preparing a high-entropy alloy/carbon nanotube composite material, which comprises the following specific steps:
step 1.1, respectively weighing an iron source, a cobalt source, a copper source, a zinc source, an indium source, a nickel source and a carbon source according to the molar ratio of iron, cobalt, copper, zinc, indium, nickel and carbon atoms of (0.1-1): 5-20): 20-50, mixing, adding into a mortar, and grinding to uniformly mix to obtain a mixture A;
step 1.2, placing the mixture A into a high-temperature tube furnace, heating the mixture A from room temperature to 180 ℃ at a heating rate of 10-30 ℃/min under an inert atmosphere, and then preserving heat for 0.5-2 h;
step 1.3, closing the high-temperature tube furnace, taking out after the temperature in the furnace is reduced to room temperature, sealing the furnace in a glass bottle filled with argon through a glove box, putting the glass bottle into a microwave synthesis instrument, and reacting for 5-10min at 800-;
step 1.4, after the reaction is finished, cooling the mixture to room temperature and then taking the mixture out to obtain the high-entropy alloy/carbon nano tube composite material;
step 2, weighing 70-90% of carbon fluoride, 5-20% of high-entropy alloy/carbon nanotube composite material and 5-10% of binder according to mass percent, grinding and mixing uniformly, then adding a solvent, and stirring uniformly to obtain a positive electrode slurry with fluidity;
and 3, uniformly coating the positive electrode slurry on an aluminum foil or a carbon-coated aluminum foil by using a film coater, and drying and removing the solvent in vacuum to obtain the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive electrode sheet.
Further, the iron source in step 1.1 is one or a combination of any several of ferrous ammonium sulfate, ferrous chloride, ammonium ferric oxalate or ferric citrate;
the cobalt source is one or the combination of any more of cobalt nitrate, cobalt carbonate or cobalt sulfate;
the copper source is one or the combination of any more of cuprous chloride, copper sulfate or copper nitrate;
the zinc source is zinc acetate, zinc sulfate or the combination of zinc acetate and zinc sulfate;
the indium source is indium nitrate, indium sulfate or a combination of indium nitrate and indium sulfate;
the nickel source is one or the combination of any more of nickel sulfate, nickel nitrate, nickel chloride, nickel sulfamate, nickel bromide or nickel hydroxide;
the carbon source is one or the combination of any of urea, melamine or glucose.
Further, the binder in step 2 is polyvinylidene fluoride, hydroxymethyl cellulose, polyacrylic acid or a mixture of hydroxymethyl cellulose and polyacrylic acid.
Further, the step 3 adopts a vacuum drying oven to dry for 10-14h at 70-90 ℃.
Further, when the binder in the step 2 is polyvinylidene fluoride, the solvent is N-methyl pyrrolidone or N, N-dimethylformamide; when the binder in the step 2 is hydroxymethyl cellulose, polyacrylic acid or a mixture of hydroxymethyl cellulose and polyacrylic acid, the solvent is deionized water.
The invention also relates to the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate prepared by the method, which is characterized by comprising a positive current collector and an active coating coated on the positive current collector;
the positive current collector is an aluminum foil or a carbon-coated aluminum foil;
the active coating comprises 70-90% of carbon fluoride, 5-20% of high-entropy alloy/carbon nanotube composite material and 5-10% of binder by mass percent.
The invention also provides a lithium fluorocarbon battery prepared by the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate, which comprises electrolyte, a diaphragm, a negative plate and the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate.
Further, the diaphragm is a polyethylene sheet, a polypropylene sheet or a multilayer composite diaphragm.
Further, the electrolyte of the electrolyte is LiTFSI and LiClO4Or one or the combination of any several of LiPF6, and the solvent of the electrolyte is one or the combination of any several of PC, EC, DEC, DMC or EMC.
Compared with the prior art, the invention has the following technical effects:
according to the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate, due to the addition of the high-entropy alloy/carbon nanotube composite material rich in active sites, good conductivity is provided, meanwhile, a plurality of active sites are provided for the positive plate, a catalytic effect is achieved, and the electrochemical reaction activity is improved; the lithium fluorocarbon battery prepared by the positive plate has a high voltage platform and platform stability, and the rate capability of the battery can be improved.
Drawings
FIG. 1 is an XRD pattern of the high-entropy alloy/carbon nanotube composite material prepared in example 1 of the present invention;
FIG. 2 is a Transmission Electron Microscope (TEM) image of the high-entropy alloy/carbon nanotube composite material prepared in example 1 of the present invention;
FIG. 3 is an SEM photograph of carbon fluoride used in example 1 of the present invention;
fig. 4 is a graph of electrochemical performance of a lithium fluorocarbon cell provided in example 7 of the present invention under 1C test conditions.
Detailed Description
The present invention will be explained in further detail with reference to examples.
The embodiment provides a preparation method of a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate, which comprises the following steps:
step 1, preparing a high-entropy alloy/carbon nanotube composite material, which comprises the following specific steps:
step 1.1, respectively weighing an iron source, a cobalt source, a copper source, a zinc source, an indium source, a nickel source and a carbon source according to the molar ratio of iron, cobalt, copper, zinc, indium, nickel and carbon atoms of (0.1-1): 5-20): 20-50, mixing, adding into a mortar, and grinding to uniformly mix to obtain a mixture A;
step 1.2, placing the mixture A into a high-temperature tube furnace, heating the mixture A from room temperature to 180 ℃ at a heating rate of 10-30 ℃/min under an inert atmosphere, and then preserving heat for 0.5-2 h;
step 1.3, closing the high-temperature tube furnace, taking out after the temperature in the furnace is reduced to room temperature, sealing the furnace in a glass bottle filled with argon through a glove box, putting the glass bottle into a microwave synthesis instrument, and reacting for 5-10min at 800-;
step 1.4, after the reaction is finished, cooling the mixture to room temperature and then taking the mixture out to obtain the high-entropy alloy/carbon nano tube composite material;
step 2, weighing 70-90% of carbon fluoride, 5-20% of high-entropy alloy/carbon nanotube composite material and 5-10% of binder according to mass percent, grinding and mixing uniformly, then adding a solvent, and stirring uniformly to obtain a positive electrode slurry with fluidity;
and 3, uniformly coating the positive electrode slurry on an aluminum foil or a carbon-coated aluminum foil by using a film coater, and drying and removing the solvent in vacuum to obtain the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive electrode sheet.
The embodiment also provides a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate prepared by the method, which comprises a positive current collector and an active coating coated on the positive current collector;
the positive current collector is an aluminum foil or a carbon-coated aluminum foil;
the active coating comprises 70-90% of carbon fluoride, 5-20% of high-entropy alloy/carbon nanotube composite material and 5-10% of binder by mass percent.
The embodiment also relates to a lithium fluorocarbon battery prepared by the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate, which comprises electrolyte, a diaphragm, a negative plate and the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate.
To further illustrate the technical solution of the present invention, the following detailed description is given with reference to specific examples.
Example 1
A preparation method of a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate comprises the following steps:
step 1, preparing a high-entropy alloy/carbon nanotube composite material, which comprises the following specific steps:
step 1.1, according to the mole ratio of iron, cobalt, copper, zinc, indium, nickel and carbon atoms of 0.1: 0.128: 0.155: 0.17: 0.124: 5.78: 24.78 ammonium oxalate ferric salt, cobalt nitrate, copper nitrate, zinc acetate, indium nitrate, nickel nitrate hexahydrate and melamine are respectively weighed, mixed and then added into an agate mortar, and ground for 20min to be uniformly mixed, so as to obtain a mixture A;
step 1.2, placing the mixture A into a high-temperature tubular furnace, heating the mixture A from room temperature to 180 ℃ at a heating rate of 30 ℃/min under a nitrogen atmosphere of 80sccm, and then preserving heat for 0.5 h;
step 1.3, closing the high-temperature tube furnace, taking out after the temperature in the furnace is reduced to room temperature, sealing the furnace in a glass bottle filled with argon through a glove box, putting the glass bottle into a microwave synthesis instrument, and reacting for 5min at 1000K;
step 1.4, after the reaction is finished, cooling the mixture to room temperature and then taking the mixture out to obtain the high-entropy alloy/carbon nano tube composite material;
step 2, weighing 70% of carbon fluoride, 20% of high-entropy alloy/carbon nanotube composite material and 10% of polyvinylidene fluoride according to mass percentage, uniformly grinding, adding N-methyl pyrrolidone, and uniformly stirring to obtain anode slurry;
and 3, uniformly coating the positive electrode slurry on an aluminum foil by using a film coater, and drying for 12 hours in a vacuum drying oven at the temperature of 80 ℃ to obtain the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive electrode sheet.
FIG. 1 is an XRD pattern of the high-entropy alloy/carbon nanotube composite material prepared in the present example; it is clear from the figure that the carbon peak exists at 25.95 degrees of 2 theta, the diffraction peaks which exist at 44.3 degrees and 51.6 degrees are high-entropy alloy, and the crystallinity is better and the peak intensity is high.
FIG. 2 is a Transmission Electron Microscope (TEM) image of the high-entropy alloy/carbon nanotube composite material prepared in this example; the size of the high-entropy alloy/carbon nanotube composite material is about 200nm, the appearance is complete, and the surface of the carbon nanotube has a large number of folds, so that the specific surface area is increased, and the high-entropy alloy/carbon nanotube composite material has rich active sites.
FIG. 3 is an SEM photograph of fluorocarbon used in the present example; it can be seen that the carbon fluoride material selected is a lamellar structure.
Example 2
A preparation method of a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate comprises the following steps:
step 1, preparing a high-entropy alloy/carbon nanotube composite material, which comprises the following specific steps:
step 1.1, weighing ammonium ferrous sulfate, cobalt carbonate, cuprous chloride, zinc sulfate, indium sulfate, nickel sulfate and urea respectively according to the molar ratio of iron to cobalt to copper to zinc to indium to nickel to carbon of 1:1:1:0.1:0.1:5:20, mixing, adding into an agate mortar, grinding for 15min, and uniformly mixing to obtain a mixture A;
step 1.2, placing the mixture A into a high-temperature tube furnace, heating the mixture A from room temperature to 150 ℃ at a heating rate of 10 ℃/min in a nitrogen atmosphere of 120sccm, and then preserving heat for 2 hours;
step 1.3, closing the high-temperature tube furnace, taking out after the temperature in the furnace is reduced to room temperature, sealing the furnace in a glass bottle filled with argon through a glove box, putting the glass bottle into a microwave synthesis instrument, and reacting for 10min at 800K;
step 1.4, after the reaction is finished, cooling the mixture to room temperature and then taking the mixture out to obtain the high-entropy alloy/carbon nano tube composite material;
step 2, weighing 90% of carbon fluoride, 5% of high-entropy alloy/carbon nanotube composite material and 5% of hydroxymethyl cellulose (CMC) according to mass percentage, uniformly grinding, adding deionized water, and uniformly stirring to obtain anode slurry;
and 3, uniformly coating the positive electrode slurry on the carbon-coated aluminum foil by using a film coater, and drying for 14 hours in a vacuum drying oven at 70 ℃ to obtain the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive electrode sheet.
Example 3
A preparation method of a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate comprises the following steps:
step 1, preparing a high-entropy alloy/carbon nanotube composite material, which comprises the following specific steps:
step 1.1, respectively weighing an iron source, a cobalt source, a copper source, a zinc source, an indium source, a nickel source and a carbon source according to the molar ratio of iron to cobalt to copper to zinc to indium to nickel to carbon to be 0.1:0.2:0.2:0.2: 20:50, mixing, adding into an agate mortar, wherein the iron source is ferrous sulfate and ferric citrate with the molar ratio of iron to iron being 1:1, the cobalt source is cobalt nitrate and cobalt carbonate with the molar ratio of cobalt to cobalt being 1:1, and the copper source is copper to carbon with the molar ratio of 1:2, cuprous chloride and cupric nitrate, and zinc source is a zinc source with the molar ratio of zinc atoms being 1:1, the indium source is an indium source with an indium atom molar ratio of 2: 1, and the nickel source is nickel atom with the molar ratio of 1:1, nickel nitrate and nickel sulfamate, wherein the carbon source is a carbon source with the carbon atom molar ratio of 1:2, grinding the melamine and the urea for 18min to uniformly mix the melamine and the urea to obtain a mixture A;
step 1.2, placing the mixture A into a high-temperature tube furnace, heating the mixture A from room temperature to 160 ℃ at a heating rate of 20 ℃/min under an argon atmosphere of 100sccm, and then preserving heat for 1 h;
step 1.3, closing the high-temperature tube furnace, taking out after the temperature in the furnace is reduced to room temperature, sealing the furnace in a glass bottle filled with argon through a glove box, putting the glass bottle into a microwave synthesis instrument, and reacting for 7min at 900K;
step 1.4, after the reaction is finished, cooling the mixture to room temperature and then taking the mixture out to obtain the high-entropy alloy/carbon nano tube composite material;
step 2, weighing 80% of carbon fluoride, 10% of high-entropy alloy/carbon nanotube composite material and 10% of polyacrylic acid (PAA) according to mass percentage, uniformly grinding, adding deionized water, and uniformly stirring to obtain anode slurry;
and 3, uniformly coating the positive electrode slurry on the carbon-coated aluminum foil by using a film coater, and drying for 10 hours in a vacuum drying oven at 90 ℃ to obtain the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive electrode sheet.
Example 4
The high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate prepared by the method in the embodiment 1 comprises a positive current collector and an active coating coated on the positive current collector; wherein, the positive current collector is aluminum foil, and the active coating comprises 70% of carbon fluoride, 20% of high-entropy alloy/carbon nanotube composite material and 10% of polyvinylidene fluoride (PVDF) in percentage by mass.
Example 5
The high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate prepared by the method in the embodiment 2 comprises a positive current collector and an active coating coated on the positive current collector; the positive current collector is a carbon-coated aluminum foil, and the active coating comprises 90% of carbon fluoride, 5% of high-entropy alloy/carbon nanotube composite material and 5% of hydroxymethyl cellulose (CMC) in percentage by mass.
Example 6
The high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate prepared by the method in the embodiment 3 comprises a positive current collector and an active coating coated on the positive current collector; the positive electrode current collector is a carbon-coated aluminum foil, and the active coating comprises 80 mass percent of carbon fluoride, 10 mass percent of high-entropy alloy/carbon nanotube composite material and 10 mass percent of polyacrylic acid (PAA).
Example 7
A lithium fluorocarbon battery comprises electrolyte, a diaphragm, a negative plate and the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate prepared in example 1, wherein electrolyte of the electrolyte is LiPF6, a solvent is EC, the diaphragm is a polypropylene plate, and the negative plate is metallic lithium.
Fig. 4 is a graph of electrochemical performance of the lithium fluorocarbon cell provided in this example under 1C test conditions; it is seen that the lithium fluorocarbon cell presents a high voltage plateau around 2.35V and provides specific capacity of 708.1mAh/g over the voltage range of 3V-1.5V; therefore, the lithium-carbon fluoride battery prepared by the high-entropy alloy/carbon nanotube modified lithium-carbon fluoride battery positive plate has high capacity, a high-voltage platform is more stable, and the electrochemical reaction is stable.
Example 8
A lithium fluorocarbon battery comprises electrolyte, a diaphragm, a negative plate and the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate prepared in example 2, wherein the electrolyte of the electrolyte is LiClO4The solvent is DEC and DMC with the volume ratio of 1:2, the diaphragm is a polyethylene sheet, and the negative plate is metal lithium.
Example 9
A lithium fluorocarbon battery comprises electrolyte, a diaphragm, a negative plate and the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate prepared in example 3, wherein the electrolyte of the electrolyte is LiPF6 and LiClO in a mass ratio of 1:14The solvent is PC, the diaphragm is a multilayer composite diaphragm, and the negative plate is metallic lithium.
Claims (9)
1. A preparation method of a high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate is characterized by comprising the following steps:
step 1, preparing a high-entropy alloy/carbon nanotube composite material, which comprises the following specific steps:
step 1.1, respectively weighing an iron source, a cobalt source, a copper source, a zinc source, an indium source, a nickel source and a carbon source according to the molar ratio of iron, cobalt, copper, zinc, indium, nickel and carbon atoms of (0.1-1): 5-20): 20-50, mixing, adding into a mortar, and grinding to uniformly mix to obtain a mixture A;
step 1.2, placing the mixture A into a high-temperature tube furnace, heating the mixture A from room temperature to 180 ℃ at a heating rate of 10-30 ℃/min under an inert atmosphere, and then preserving heat for 0.5-2 h;
step 1.3, closing the high-temperature tube furnace, taking out after the temperature in the furnace is reduced to room temperature, sealing the furnace in a glass bottle filled with argon through a glove box, putting the glass bottle into a microwave synthesis instrument, and reacting for 5-10min at 800-;
step 1.4, after the reaction is finished, cooling the mixture to room temperature and then taking the mixture out to obtain the high-entropy alloy/carbon nano tube composite material;
step 2, weighing 70-90% of carbon fluoride, 5-20% of high-entropy alloy/carbon nanotube composite material and 5-10% of binder according to mass percent, grinding and mixing uniformly, then adding a solvent, and stirring uniformly to obtain a positive electrode slurry with fluidity;
and 3, uniformly coating the positive electrode slurry on an aluminum foil or a carbon-coated aluminum foil by using a film coater, and drying and removing the solvent in vacuum to obtain the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive electrode sheet.
2. The method for preparing the high-entropy alloy/carbon nanotube modified lithium carbon fluoride battery positive plate as claimed in claim 1, wherein the iron source in the step 1.1 is one or a combination of any more of ammonium ferrous sulfate, ferrous chloride, ferric ammonium oxalate and ferric citrate;
the cobalt source is one or the combination of any more of cobalt nitrate, cobalt carbonate or cobalt sulfate;
the copper source is one or the combination of any more of cuprous chloride, copper sulfate or copper nitrate;
the zinc source is zinc acetate, zinc sulfate or the combination of zinc acetate and zinc sulfate;
the indium source is indium nitrate, indium sulfate or a combination of indium nitrate and indium sulfate;
the nickel source is one or the combination of any more of nickel sulfate, nickel nitrate, nickel chloride, nickel sulfamate, nickel bromide or nickel hydroxide;
the carbon source is one or the combination of any of urea, melamine or glucose.
3. The method for preparing the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate as claimed in claim 1, wherein the binder in the step 2 is polyvinylidene fluoride, hydroxymethyl cellulose, polyacrylic acid or a mixture of hydroxymethyl cellulose and polyacrylic acid.
4. The preparation method of the high-entropy alloy/carbon nanotube modified lithium-carbon fluoride battery positive plate as claimed in claim 1, wherein the vacuum drying in the step 3 is performed for 10-14h at 70-90 ℃ by using a vacuum drying oven.
5. The preparation method of the high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate as claimed in claim 3, wherein when the binder in the step 2 is polyvinylidene fluoride, the solvent is N-methylpyrrolidone or N, N-dimethylformamide; when the binder in the step 2 is hydroxymethyl cellulose, polyacrylic acid or a mixture of hydroxymethyl cellulose and polyacrylic acid, the solvent is deionized water.
6. The high-entropy alloy/carbon nanotube modified lithium fluorocarbon battery positive plate prepared by the method of claim 1, which comprises a positive current collector and an active coating coated on the positive current collector;
the positive current collector is an aluminum foil or a carbon-coated aluminum foil;
the active coating comprises 70-90% of carbon fluoride, 5-20% of high-entropy alloy/carbon nanotube composite material and 5-10% of binder by mass percent.
7. The lithium-carbon fluoride battery prepared from the high-entropy alloy/carbon nanotube modified lithium-carbon fluoride battery positive plate as claimed in claim 6, is characterized by comprising an electrolyte, a diaphragm, a negative plate and the high-entropy alloy/carbon nanotube modified lithium-carbon fluoride battery positive plate.
8. The lithium fluorocarbon cell of claim 7, wherein the separator is a polyethylene sheet, a polypropylene sheet, or a multilayer composite separator.
9. The lithium fluorinated carbon cell of claim 7,
the electrolyte of the electrolyte is LiTFSI and LiClO4Or LiPF6The solvent of the electrolyte is one or the combination of any of PC, EC, DEC, DMC or EMC.
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