CN114613974A - Long-life quick-charging type lithium ion battery cathode material and preparation method thereof - Google Patents
Long-life quick-charging type lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN114613974A CN114613974A CN202210400788.XA CN202210400788A CN114613974A CN 114613974 A CN114613974 A CN 114613974A CN 202210400788 A CN202210400788 A CN 202210400788A CN 114613974 A CN114613974 A CN 114613974A
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- ion battery
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- lithium ion
- cerium
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 38
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000010406 cathode material Substances 0.000 title claims description 19
- 229910021385 hard carbon Inorganic materials 0.000 claims abstract description 56
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 229910021384 soft carbon Inorganic materials 0.000 claims abstract description 21
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 20
- 239000007833 carbon precursor Substances 0.000 claims abstract description 19
- 239000007773 negative electrode material Substances 0.000 claims abstract description 19
- 239000013589 supplement Substances 0.000 claims abstract description 19
- QCCDYNYSHILRDG-UHFFFAOYSA-K cerium(3+);trifluoride Chemical compound [F-].[F-].[F-].[Ce+3] QCCDYNYSHILRDG-UHFFFAOYSA-K 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 11
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 11
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 11
- 239000011737 fluorine Substances 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000006258 conductive agent Substances 0.000 claims abstract description 9
- 239000010426 asphalt Substances 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000004108 freeze drying Methods 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 23
- 229910020187 CeF3 Inorganic materials 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 8
- 229910010699 Li5FeO4 Inorganic materials 0.000 claims description 7
- 238000003763 carbonization Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 229910008722 Li2NiO2 Inorganic materials 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 6
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000007784 solid electrolyte Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 229910001323 Li2O2 Inorganic materials 0.000 claims description 4
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 4
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 4
- MOOUSOJAOQPDEH-UHFFFAOYSA-K cerium(iii) bromide Chemical compound [Br-].[Br-].[Br-].[Ce+3] MOOUSOJAOQPDEH-UHFFFAOYSA-K 0.000 claims description 4
- 229920000620 organic polymer Polymers 0.000 claims description 4
- 235000003270 potassium fluoride Nutrition 0.000 claims description 4
- 239000011698 potassium fluoride Substances 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 3
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 3
- 244000060011 Cocos nucifera Species 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 3
- 229920005546 furfural resin Polymers 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
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- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 235000013024 sodium fluoride Nutrition 0.000 claims description 3
- 239000011775 sodium fluoride Substances 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
- 239000002224 Li5La3Nb2O12 Substances 0.000 claims description 2
- 229910010709 Li5La3Nb2O12 Inorganic materials 0.000 claims description 2
- 239000002225 Li5La3Ta2O12 Substances 0.000 claims description 2
- 229910010712 Li5La3Ta2O12 Inorganic materials 0.000 claims description 2
- 229910010629 Li6.75La3Zr1.75Nb0.25O12 Inorganic materials 0.000 claims description 2
- 229910002984 Li7La3Zr2O12 Inorganic materials 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 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
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 229920005610 lignin Polymers 0.000 claims description 2
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 2
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 239000011257 shell material Substances 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 229930192474 thiophene Natural products 0.000 claims description 2
- 230000001502 supplementing effect Effects 0.000 claims 1
- 239000011230 binding agent Substances 0.000 abstract description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000005056 compaction Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- -1 stirring and pulping Substances 0.000 description 4
- 229910001290 LiPF6 Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- 239000000654 additive Substances 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910013716 LiNi Inorganic materials 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- 229910021543 Nickel dioxide Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 239000002194 amorphous carbon material Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/00—Electrodes
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- 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)
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- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
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- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention disclosesA long-life quick-charging type lithium ion battery negative electrode material is prepared from hard carbon and CeF coated on its external layer3And soft carbon of a lithium supplement agent, wherein the mass ratio of the outer layer is 1-10% and the soft carbon is 1-10% of CeF (CeF)31-10% of lithium supplement agent and 80-98% of soft carbon. The preparation method comprises the steps of adding a cerium source, a fluorine source, a nitrogen source and a conductive agent into an organic solvent, performing hydrothermal reaction and freeze drying to obtain porous cerium fluoride, uniformly mixing the porous cerium fluoride with an asphalt binder and a lithium supplement agent, performing ball milling, mixing with a hard carbon precursor, and carbonizing to obtain the composite material. The invention can improve the first efficiency, the dynamics and the cycle performance of the hard carbon.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery materials, particularly relates to a long-life quick-charging type lithium ion battery cathode material, and also relates to a preparation method of the long-life quick-charging type lithium ion battery cathode material.
Background
Hard carbon is a non-graphitizable carbon material and has the advantages of excellent quick charge, low temperature, rate cycle, low expansion and the like, but has the defects of low efficiency for the first time, poor high-temperature storage and the like. At present, the measures for improving the first efficiency and the high-temperature performance of the hard carbon material mainly comprise soft carbon coating and lithium supplement of the material, but the rate performance is reduced due to the fact that the dynamic performance of the material is reduced after the coating. For example, chinese patent 202110968525.4 discloses a fast-charging high-efficiency hard carbon/artificial graphite negative electrode material and a preparation method thereof, wherein the preparation method comprises: crushing the hard carbon material, then uniformly mixing the crushed hard carbon material with a coating agent, carrying out heat treatment to prepare a coated hard carbon material, and carrying out high-temperature heat treatment to prepare the high-first-efficiency hard carbon artificial graphite cathode material. Although the first efficiency of the material is improved, the rate capability and the cycle performance of the material are reduced. One of the measures for improving the dynamic performance and the cycle performance of the material after being coated is to supplement enough lithium ions and a stabilizing additive with a stable material structure in the charging and discharging process, so that the first efficiency and the dynamic performance of the material can be improved on one hand, and the additive has the characteristics of good electrolyte compatibility and stable structure on the other hand, and the side reaction in the charging and discharging process can be reduced.
Disclosure of Invention
The invention aims to overcome the defects and provide a long-life quick-charging type lithium ion battery cathode material which can improve the first efficiency, the dynamics and the cycle performance of hard carbon.
The invention also aims to provide a preparation method of the long-life quick-charging lithium ion battery negative electrode material.
The invention relates to a long-life quick-charging lithium ion battery cathode material which is made of hard carbon and contains CeF coated on the outer layer3And soft carbon of a lithium supplement agent, wherein the mass of the negative electrode material is 100%, and the mass ratio of the outer layer is 1-10%.
The outer layer is made of 1-10% CeF31-10% of lithium supplement agent and 80-98% of soft carbon, wherein: the lithium supplement agent is Li2NiO2、Li5FeO4、Li3N、Li2O2Or Li2And (5) one of S.
The invention relates to a preparation method of a long-life quick-charging type lithium ion battery cathode material, which comprises the following steps:
(1) preparation of hard carbon precursor:
according to the following steps of 100: 0.5-2: adding an organic polymer, phosphoric acid and a solid electrolyte into an organic solvent according to a mass ratio of 0.5-2 to prepare a mixture with a mass concentration of 5-20%, uniformly stirring, transferring the mixture into a high-pressure reaction kettle to perform hydrothermal reaction for 6 hours at 150 ℃, filtering, and performing vacuum drying for 24 hours at 80 ℃ to obtain a hard carbon precursor;
(2) preparation of porous cerium fluoride:
weighing a cerium source and a fluorine source according to a molar ratio Ce to halogen elements of 1:3, adding the cerium source and the fluorine source into polyethylene glycol to prepare a 1-10 wt% solution, and mixing the cerium source and the fluorine source according to the weight ratio of a nitrogen source: conductive agent: adding a nitrogen source and a conductive agent into the mixture according to the mass ratio of (a cerium source and a fluorine source) of 1-10: 100, ultrasonically dispersing the mixture for 1h at 20KHZ and 120W, uniformly performing hydrothermal reaction at 150 ℃ for 6h, and freeze-drying the mixture for 24h at-40 ℃ to obtain porous cerium fluoride;
(3) preparing a soft carbon-coated hard carbon composite material:
mixing a hard carbon precursor, porous cerium fluoride, a lithium supplement agent and asphalt in a mass ratio of 100: 0.1 to 1; 0.1-1: ball-milling the mixture to a particle size of 5-20 microns by 1-10 balls, uniformly mixing, heating to 150-250 ℃ under the protection of Ar gas for coating, and heating to 900-1200 ℃ for carbonization for 3 hours to obtain the product.
The preparation method of the long-life quick-charging lithium ion battery cathode material comprises the following steps: the organic polymer in the step (1) is one of phenolic resin, furfural resin, epoxy resin, coconut shell, starch, glucose, sucrose, lignin or cellulose.
The long-life quick charging typeThe preparation method of the lithium ion battery negative electrode material comprises the following steps: the solid electrolyte in the step (1) is Li7La3Zr2O12、Li6.75La3Zr1.75Nb0.25O12、Li5La3Nb2O12Or Li5La3Ta2O12One kind of (1).
The preparation method of the long-life quick-charging lithium ion battery cathode material comprises the following steps: the organic solvent in the step (1) is one of ethanol, isopropanol, acetone or dimethylformamide.
The preparation method of the long-life quick-charging lithium ion battery cathode material comprises the following steps: the cerium source in the step (2) is one of cerium chloride, cerium bromide, cerium nitrate or cerium sulfate.
The preparation method of the long-life quick-charging lithium ion battery cathode material comprises the following steps: the fluorine source in the step (2) is one of sodium fluoride, potassium fluoride, calcium fluoride, magnesium fluoride or ammonium fluoride.
The preparation method of the long-life quick-charging lithium ion battery cathode material comprises the following steps: and (3) the nitrogen source in the step (2) is one of aniline, urea, melamine, pyrrole or thiophene.
The preparation method of the long-life quick-charging lithium ion battery cathode material comprises the following steps: the lithium supplement agent in the step (3) is Li2NiO2、Li5FeO4、Li3N、Li2O2Or Li2And (5) one of S.
Compared with the prior art, the invention has obvious beneficial effects, and the technical scheme can show that: the invention coats a lithium supplement agent and CeF on the surface of hard carbon3The amorphous carbon material exerts the synergistic effect of the three materials, and the lithium supplement agent provides sufficient lithium ions in the charge and discharge process to reduce the irreversible loss of the negative electrode material and improve the multiplying power and the cycle performance; CeF3Is porous structure, restrains the expansion of the material in the charging and discharging process and stabilizes the structural stability of the material, and has better compatibility with the electrolyteSimultaneously porous CeF3Improvement of CeF by doping with nitrogen atoms and its conductive agent3Poor self-electron conductivity and the like; the amorphous carbon has low electron impedance, good fluidity in molten state, and excellent processability, and can be used in combination with lithium supplement agent and CeF3The core hard carbon material is uniformly coated on the surface of the core hard carbon material, so that the first efficiency and the power performance of the core hard carbon material are improved. The solid electrolyte is contained in the core, so that the transmission rate and the conductivity of lithium ions in the charge and discharge process of the core can be improved, and the multiplying power and the cycle performance are improved.
Drawings
Fig. 1 is an SEM image of a hard carbon composite prepared in example 1.
Detailed Description
Example 1:
a preparation method of a long-life quick-charging type lithium ion battery cathode material comprises the following steps:
(1) preparation of hard carbon precursor:
100g of phenolic resin, 1g of phosphoric acid and 1gLi7La3Zr2O12Adding the solution into 1020ml of isopropanol solvent to prepare 10% concentration, uniformly stirring, transferring the solution into a high-pressure reaction kettle to perform hydrothermal reaction (the temperature is 150 ℃ and 6 hours), filtering, and performing vacuum drying at 80 ℃ for 24 hours to obtain a hard carbon precursor;
(2) preparation of porous cerium fluoride material:
weighing 24.6g of cerium chloride (0.1mol) and 12.6g of sodium fluoride (0.3mol), adding the mixture into 744ml of polyethylene glycol to prepare a 5 wt% solution, then adding 1.86g of aniline and 1.86g of carbon nano tubes, uniformly dispersing the mixture in ultrasonic (20KHZ, 120W, 1h), and then carrying out hydrothermal reaction (the temperature is 150 ℃, 6h) and freeze-drying at-40 ℃ for 24h to obtain a porous cerium fluoride material;
(3) preparing a soft carbon-coated hard carbon composite material:
100g of hard carbon precursor, 0.5g of porous cerium fluoride, 0.5g of 0.5gLi5FeO4And 5g of asphalt is evenly mixed by ball milling, firstly heated to 200 ℃ for coating under the protection of Ar gas, and then heated to 1000 ℃ for carbonization for 3h to obtain the product containing CeF3/Li5FeO4Soft carbon coated hard carbon compositeThe composite material comprises hard carbon and a coated outer layer, wherein the mass ratio of the outer layer is 8% and the outer layer is 2% CeF (CeF) based on 100% of the mass3、2％Li5FeO496% soft carbon.
Example 2:
a preparation method of a long-life quick-charging type lithium ion battery cathode material comprises the following steps:
(1) preparation of hard carbon precursor:
mixing 100g of furfural resin, 0.5g of phosphoric acid and 0.5g of 0.5gLi6.75La3Zr1.75Nb0.25O12Adding the mixture into 2020ml of ethanol solvent to prepare 5% of concentration, uniformly stirring, transferring the mixture into a high-pressure reaction kettle to perform hydrothermal reaction (the temperature is 150 ℃ and 6 hours), filtering, and performing vacuum drying at 80 ℃ for 24 hours to obtain a hard carbon precursor;
(2) preparation of porous cerium fluoride material:
weighing 37.9g of cerium bromide (0.1mol) and 17.4g of potassium fluoride (0.3mol), adding the cerium bromide and the potassium fluoride into 5530ml of polyethylene glycol to prepare a1 wt% solution, then adding 0.55g of urea and 0.55g of graphene, uniformly dispersing the mixture in ultrasonic (20KHZ, 120W and 1h), and then carrying out hydrothermal reaction (the temperature is 150 ℃, 6h) and freeze-drying at-40 ℃ for 24h to obtain a porous cerium fluoride material;
(3) preparing a soft carbon-coated hard carbon composite material:
100g of hard carbon precursor, 0.1g of porous cerium fluoride, 0.1g of 0.1gLi2NiO2And 1g of asphalt is added into the mixture and is evenly mixed by ball milling, under the protection of Ar gas, the mixture is firstly heated to 150 ℃ for softening and coating, and then heated to 900 ℃ for carbonization for 3h to obtain the product containing CeF3/Li2NiO2The soft carbon-coated hard carbon composite material comprises hard carbon and a coated outer layer, wherein the mass ratio of the outer layer is 1% and the mass ratio of the outer layer is 1% by mass and the outer layer is 1% CeF (CeF)3、1％Li2NiO298% soft carbon.
Example 3:
(1) preparation of hard carbon precursor:
mixing 100g of coconut shell, 2g of phosphoric acid, 2gLi5La3Nb2O12Added into 520ml of acetone flux to prepareUniformly stirring the mixture with the concentration of 20%, transferring the mixture into a high-pressure reaction kettle to perform hydrothermal reaction (the temperature is 150 ℃ and 6 hours), filtering, and performing vacuum drying at the temperature of 80 ℃ for 24 hours to obtain a hard carbon precursor;
(2) preparation of porous cerium fluoride material:
weighing 43.4g of cerium nitrate (0.1mol) and 11.1g of ammonium fluoride (0.3mol), adding the mixture into 545ml of polyethylene glycol to prepare a10 wt% solution, then adding 5.45g of melamine and 5.45g of carbon black, uniformly dispersing by ultrasonic, and then carrying out hydrothermal reaction (at the temperature of 150 ℃, 6h) and freeze-drying at the temperature of-40 ℃ for 24h to obtain a porous cerium fluoride material;
(3) preparing a soft carbon-coated hard carbon composite material:
100g of a hard carbon precursor, 1g of porous cerium fluoride, 1gLi3After N and 8g of asphalt are ball-milled and mixed uniformly, under the protection of Ar gas, the temperature is firstly raised to 250 ℃ for softening and coating, and then the temperature is raised to 1200 ℃ for carbonization for 1h to obtain the product containing CeF3/Li3The N soft carbon-coated hard carbon composite material comprises hard carbon and a coated outer layer, wherein the mass ratio of the outer layer is 10% and the outer layer is 10% CeF (CeF)3、10％Li3N, 80% soft carbon.
Comparative example 1:
the hard carbon precursor obtained in the step (1) in example 1 was used and carbonized at 1000 ℃ for 3 hours in an argon atmosphere to obtain a hard carbon composite material.
Comparative example 2
100g of the hard carbon precursor in step (1) of example 1, 0.5gLi, was taken5FeO4And 5g of asphalt is subjected to ball milling and uniform mixing, firstly heated to 200 ℃ for softening and coating under the protection of Ar gas, and then heated to 1000 ℃ for carbonization for 3h to obtain the product containing Li5FeO4The soft carbon of (a) coats the hard carbon composite material.
Comparative example 3
Taking 100g of hard carbon precursor, 0.5g of porous cerium fluoride and 5g of pitch in the step (1) in the example 1, ball-milling and uniformly mixing, firstly heating to 200 ℃ for softening and coating under the protection of Ar gas, then heating to 1000 ℃ for carbonization for 3h to obtain the product containing CeF3The soft carbon of (a) coats the hard carbon composite material.
1. Physical and chemical property test
1.1SEM test
The hard carbon composite material prepared in example 1 was subjected to SEM test, and the test results are shown in fig. 1. As can be seen from FIG. 1, the hard carbon composite material prepared in example 1 has a granular structure, is slightly granulated, has a uniform size distribution, and has a particle size of 3-8 μm. 1.2 powder conductivity test:
pressing the powder into a blocky structure, and then testing the conductivity of the powder by adopting a four-probe tester. The test results are shown in table 1.
1.3 powder compaction Density test
The hard carbon composites prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to a powder compaction density test. During testing, powder with a certain mass is weighed and placed in a mold, 2T pressure pressing is adopted (1 g of powder is placed in a fixed kettle and then pressed by 2T pressure by adopting a powder compaction density instrument, the powder is static for 10S, the volume under pressing is calculated, and the compaction density is calculated), and the powder compaction density is calculated. The test results are shown in table 1.
1.4 specific surface area and pore size test thereof
The specific surface areas and the pore diameters of the examples 1-3 and the comparative examples 1-3 are tested according to a test method in GB/T-2433and 2019 graphite cathode materials of lithium ion batteries.
TABLE 1
As can be seen from Table 1, the powder resistivity of the graphite composite materials prepared in examples 1 to 3 was significantly smaller than that of each comparative example. The reason for this is CeF3And the doped conductive agent can reduce the electronic impedance of the material; simultaneous CeF3The specific surface area of the hard carbon composite material can be improved due to the porous structure.
2. Button cell test
The composite materials in examples 1-3 and comparative examples 1-3 were assembled into button cells A1, A2, A3, B1, B2, B3. The assembling method comprises the following steps: and adding a binder, a conductive agent and a solvent into the negative electrode material, stirring and pulping, coating the mixture on copper foil, and drying and rolling to obtain the negative electrode plate. The binder used was LA132 binder, the conductive agent was SP, the negative electrode materials were the artificial graphite composite materials in examples 1 to 3 and comparative examples 1 to 3, respectively, and the solvent was double distilled water. The proportion of each component is as follows: and (3) anode material: SP: LA 132: 95g of secondary distilled water: 1 g: 4 g: 220 mL; the electrolyte is LiPF6/EC+DEC(LiPF6The concentration of the lithium ion battery is 1.2mol/L, the volume ratio of EC to DEC is 1:1), the metal lithium sheet is used as a counter electrode, and the diaphragm is a Polyethylene (PE), polypropylene (PP) or polyethylene propylene (PEP) composite membrane. The button cell is assembled in a glove box filled with argon, and the electrochemical performance test is carried out on a Wuhan blue CT2001A type battery tester, wherein the charging and discharging voltage range is 0.005V-2.0V, and the charging and discharging multiplying power is 0.1C. The test results are shown in table 2.
Meanwhile, the negative plate is taken out, and the liquid absorption capacity of the plate is tested, and the result is shown in table 2.
Table 2 button cell of examples and comparative examples and their pole piece imbibition performance comparison
As can be seen from Table 2, the lithium ion batteries using the graphite composite negative electrode materials obtained in examples 1 to 3 had significantly higher first discharge capacity, first charge-discharge efficiency, and liquid absorption capacity than the comparative examples. The lithium supplement agent releases lithium ions in the charging and discharging processes to reduce the irreversible capacity of the material surface and improve the first efficiency; meanwhile, the material in the embodiment has a high specific surface area, so that the liquid absorption performance is improved; and CeF3The method has a promoting effect on activating the activity of the hard carbon material, and further improves the specific capacity of the material.
3. Pouch cell testing
With examples 1 to 3 and comparativeThe hard carbon composite material in examples 1 to 3 was used as a negative electrode material to prepare a negative electrode sheet. With ternary materials (LiNi)1/3Co1/3Mn1/3O2) As the positive electrode, LiPF6Solution (solvent EC + DEC, volume ratio 1:1, LiPF)6Concentration 1.3mol/L) as electrolyte and celegard2400 as separator, and 2Ah soft package batteries A10, A20, A30 and B10, B20 and B30 are prepared. And testing the cycle performance and the rate performance of the soft package battery.
Multiplying power performance test conditions: charging rate: 1C/2C/3C/5C, discharge multiplying power of 1C; voltage range: 2.8-4.2V.
The cycle test conditions were 1C/1C, 2.5-4.2V, temperature: 25 +/-3 ℃ and the cycle times of 500 weeks.
The test results are shown in Table 3.
TABLE 3
As can be seen from table 3, the pouch cells prepared from the hard carbon composites prepared in examples 1 to 3 of the present invention have better constant current ratios. The constant current ratio of the comparative examples 1 to 3 is remarkably reduced, because the lithium supplement agent in the examples releases lithium ions in the charging and discharging process, the diffusion rate of the lithium ions is improved, and the multiplying power and the cycle performance are improved; simultaneous CeF3The porous structure of the material is stable, and the material is beneficial to improving the cycle performance of the material and reducing the impedance, so that the multiplying power and the cycle performance of the battery are improved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are within the scope of the present invention without departing from the technical spirit of the present invention.
Claims (10)
1. A long-life quick-charging type negative electrode material for Li-ion battery is prepared from hard carbon and CeF coated by said hard carbon3And soft carbon of lithium supplementing agent, and the negative electrode material is calculated by 100% of massThe mass ratio of the layer is 1-10%; the outer layer is made of 1-10% CeF31-10% of lithium supplement agent and 80-98% of soft carbon.
2. The long-life quick-charging lithium ion battery negative electrode material of claim 1 or 2, wherein: the lithium supplement agent is Li2NiO2、Li5FeO4、Li3N、Li2O2Or Li2And (5) one of S.
3. A preparation method of a long-life quick-charging type lithium ion battery cathode material comprises the following steps:
(1) preparation of hard carbon precursor:
according to the following steps of 100: 0.5-2: adding an organic polymer, phosphoric acid and a solid electrolyte into an organic solvent according to a mass ratio of 0.5-2 to prepare a mixture with a mass concentration of 5-20%, uniformly stirring, transferring the mixture into a high-pressure reaction kettle to perform hydrothermal reaction for 6 hours at 150 ℃, filtering, and performing vacuum drying for 24 hours at 80 ℃ to obtain a hard carbon precursor;
(2) preparation of porous cerium fluoride:
weighing a cerium source and a fluorine source according to a molar ratio Ce: halogen element =1:3, adding the cerium source and the fluorine source into polyethylene glycol to prepare a 1-10 wt% solution, and mixing the cerium source and the fluorine source according to the weight ratio of a nitrogen source: conductive agent: adding a nitrogen source and a conductive agent into the mixture according to the mass ratio of (a cerium source and a fluorine source) of 1-10: 100, ultrasonically dispersing the mixture for 1h at 20KHZ and 120W, uniformly performing hydrothermal reaction at 150 ℃ for 6h, and freeze-drying the mixture for 24h at-40 ℃ to obtain porous cerium fluoride;
(3) preparing a soft carbon-coated hard carbon composite material:
mixing a hard carbon precursor, porous cerium fluoride, a lithium supplement agent and asphalt according to a mass ratio of 100: 0.1-1: 0.1-1: ball-milling the mixture for 1-10 hours until the particle size is 5-20 mu m, uniformly mixing, heating to 150-250 ℃ under the protection of Ar gas for coating, and then heating to 900-1200 ℃ for carbonization for 3 hours to obtain the product.
4. The preparation method of the long-life quick-charging lithium ion battery negative electrode material as claimed in claim 3, wherein: the organic polymer in the step (1) is one of phenolic resin, furfural resin, epoxy resin, coconut shell, starch, glucose, sucrose, lignin or cellulose.
5. The method for preparing a long-life quick-charging lithium ion battery negative electrode material as claimed in claim 3, wherein: the solid electrolyte in the step (1) is Li7La3Zr2O12、Li6.75La3Zr1.75Nb0.25O12、Li5La3Nb2O12Or Li5La3Ta2O12One kind of (1).
6. The preparation method of the long-life quick-charging lithium ion battery negative electrode material as claimed in claim 3, wherein: the organic solvent in the step (1) is one of ethanol, isopropanol, acetone or dimethylformamide.
7. The preparation method of the long-life quick-charging lithium ion battery negative electrode material as claimed in claim 3, wherein: the cerium source in the step (2) is one of cerium chloride, cerium bromide, cerium nitrate or cerium sulfate.
8. The method for preparing the long-life quick-charging lithium ion battery cathode material as claimed in claim 3, wherein: the fluorine source in the step (2) is one of sodium fluoride, potassium fluoride, calcium fluoride, magnesium fluoride or ammonium fluoride.
9. The preparation method of the long-life quick-charging lithium ion battery negative electrode material as claimed in claim 3, wherein: and (3) the nitrogen source in the step (2) is one of aniline, urea, melamine, pyrrole or thiophene.
10. The preparation method of the long-life quick-charging lithium ion battery negative electrode material as claimed in claim 3, wherein: the lithium supplement agent in the step (3) is Li2NiO2、Li5FeO4、Li3N、Li2O2Or Li2And (5) one of S.
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Denomination of invention: A long-life fast charging lithium-ion battery negative electrode material and its preparation method Effective date of registration: 20231122 Granted publication date: 20220909 Pledgee: Guiyang Branch of Shanghai Pudong Development Bank Co.,Ltd. Pledgor: Huiyang (Guizhou) new energy materials Co.,Ltd. Registration number: Y2023520000068 |