CN106935793A - Negative pole, the method for preparing negative pole and the lithium secondary battery comprising the negative pole - Google Patents
Negative pole, the method for preparing negative pole and the lithium secondary battery comprising the negative pole Download PDFInfo
- Publication number
- CN106935793A CN106935793A CN201710133765.6A CN201710133765A CN106935793A CN 106935793 A CN106935793 A CN 106935793A CN 201710133765 A CN201710133765 A CN 201710133765A CN 106935793 A CN106935793 A CN 106935793A
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- Prior art keywords
- active material
- electrode active
- negative electrode
- material layer
- negative
- Prior art date
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- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 29
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000007773 negative electrode material Substances 0.000 claims abstract description 181
- 239000011149 active material Substances 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000003490 calendering Methods 0.000 claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 239000006183 anode active material Substances 0.000 claims abstract description 3
- 239000002002 slurry Substances 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 10
- 239000004020 conductor Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000003292 glue Substances 0.000 claims description 7
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- 229920005989 resin Polymers 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 239000010410 layer Substances 0.000 description 78
- 230000000052 comparative effect Effects 0.000 description 24
- 210000004027 cell Anatomy 0.000 description 16
- 239000011148 porous material Substances 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 10
- 239000000843 powder Substances 0.000 description 9
- -1 aluminium-cadmium Chemical compound 0.000 description 8
- 239000003792 electrolyte Substances 0.000 description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000002356 single layer Substances 0.000 description 6
- 229940084030 carboxymethylcellulose calcium Drugs 0.000 description 5
- 239000006245 Carbon black Super-P Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 238000007600 charging Methods 0.000 description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 4
- 239000005486 organic electrolyte Substances 0.000 description 4
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000003125 aqueous solvent Substances 0.000 description 3
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 description 3
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000002050 diffraction method Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000007774 positive electrode material Substances 0.000 description 3
- 238000007581 slurry coating method Methods 0.000 description 3
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- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 230000000994 depressogenic effect Effects 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910003472 fullerene Inorganic materials 0.000 description 2
- 239000006232 furnace black Substances 0.000 description 2
- 229910021385 hard carbon Inorganic materials 0.000 description 2
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
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- 239000001923 methylcellulose Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 2
- 229910021384 soft carbon Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 125000000383 tetramethylene group Chemical class [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 125000001340 2-chloroethyl group Chemical class [H]C([H])(Cl)C([H])([H])* 0.000 description 1
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical class CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 1
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 1
- 229910001558 CF3SO3Li Inorganic materials 0.000 description 1
- 229910000925 Cd alloy Inorganic materials 0.000 description 1
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical class COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 1
- 101000598921 Homo sapiens Orexin Proteins 0.000 description 1
- 101001123245 Homo sapiens Protoporphyrinogen oxidase Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910003253 LiB10Cl10 Inorganic materials 0.000 description 1
- 229910000552 LiCF3SO3 Inorganic materials 0.000 description 1
- 229910012820 LiCoO Inorganic materials 0.000 description 1
- 229910032387 LiCoO2 Inorganic materials 0.000 description 1
- 229910010584 LiFeO2 Inorganic materials 0.000 description 1
- 229910003005 LiNiO2 Inorganic materials 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
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- 102100029028 Protoporphyrinogen oxidase Human genes 0.000 description 1
- 229910006145 SO3Li Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 241001083492 Trapa Species 0.000 description 1
- 235000014364 Trapa natans Nutrition 0.000 description 1
- BEKPOUATRPPTLV-UHFFFAOYSA-N [Li].BCl Chemical compound [Li].BCl BEKPOUATRPPTLV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
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- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- DISYGAAFCMVRKW-UHFFFAOYSA-N butyl ethyl carbonate Chemical compound CCCCOC(=O)OCC DISYGAAFCMVRKW-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000006182 cathode active material Substances 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- QLVWOKQMDLQXNN-UHFFFAOYSA-N dibutyl carbonate Chemical compound CCCCOC(=O)OCCCC QLVWOKQMDLQXNN-UHFFFAOYSA-N 0.000 description 1
- 150000002012 dioxanes Chemical class 0.000 description 1
- 150000004862 dioxolanes Chemical class 0.000 description 1
- JMPVESVJOFYWTB-UHFFFAOYSA-N dipropan-2-yl carbonate Chemical compound CC(C)OC(=O)OC(C)C JMPVESVJOFYWTB-UHFFFAOYSA-N 0.000 description 1
- VUPKGFBOKBGHFZ-UHFFFAOYSA-N dipropyl carbonate Chemical compound CCCOC(=O)OCCC VUPKGFBOKBGHFZ-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910001547 lithium hexafluoroantimonate(V) Inorganic materials 0.000 description 1
- 229910001540 lithium hexafluoroarsenate(V) Inorganic materials 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 229910001537 lithium tetrachloroaluminate Inorganic materials 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- HSFDLPWPRRSVSM-UHFFFAOYSA-M lithium;2,2,2-trifluoroacetate Chemical compound [Li+].[O-]C(=O)C(F)(F)F HSFDLPWPRRSVSM-UHFFFAOYSA-M 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- KKQAVHGECIBFRQ-UHFFFAOYSA-N methyl propyl carbonate Chemical compound CCCOC(=O)OC KKQAVHGECIBFRQ-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000013612 plasmid Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 235000009165 saligot Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
-
- 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
- H01M4/043—Processes of manufacture in general involving compressing or compaction
- H01M4/0435—Rolling or calendering
-
- 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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
-
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- 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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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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Abstract
The present invention relates to negative pole, prepare the method and the lithium secondary battery comprising the negative pole of negative pole.The negative pole includes：Electrode collector；With the multilayer active material layer being formed on above-mentioned electrode collector, wherein above-mentioned multilayer active material layer is included：An anode active material layer comprising the first negative electrode active material；With the secondary negative electrode active material layer comprising the second negative electrode active material, there is relatively low compacted density and larger average particle size, wherein first negative electrode active material and the second negative electrode active material include crystalline class carbon respectively for relatively described first negative electrode active material of second negative electrode active material.Negative pole of the invention can also improve the porosity of electrode surface after calendering procedure, and can improve mobility of the ion to electrode interior, therefore, it is possible to improve the charge characteristic and life characteristic of lithium secondary battery.
Description
Present patent application is to be based on the applying date on January 22nd, 2014, entitled " negative electrode for lithium secondary battery
And the lithium secondary battery comprising the negative pole ", the divisional application of the Chinese patent application of Application No. 201480000767.2.
Technical field
Lithium secondary battery the present invention relates to negative electrode for lithium secondary battery and comprising the negative pole, more particularly, to comprising
The negative pole of the mutually different multilayer active material layer of compacted density and average particle size of negative electrode active material and negative comprising this
The lithium secondary battery of pole.
Background technology
Concern with rising, the environmental pollution of the energy prices to being caused by the exhaustion of fossil fuel increases, environmentally friendly generation
Become the indispensable factor for future life for the energy.Therefore, to using atomic energy, sunshine, wind-force and tide
The research of various Technology of Electrical Power Generation of the natural energies such as power continues, and with more effectively using producing in the above described manner
The electrical storage device of energy also gets most of the attention.
Especially, with the increase of technical research and demand to mobile device, to replacing the secondary electricity of the energy as environmental protection
The demand in pond is just sharply increased.Recently, the secondary cell needs as electric automobile (EV) or hybrid vehicle (HEV) etc.
The power source of the device of large-capacity power is used, also, as purposes such as the electric power accessory power supplys changed by grid (Grid)
And expand and use scope.
In order to be used as the power source of the device for needing the large-capacity power, powerful spy can be in a short time played
Outside property, even if while also need to be repeated in a short time with high current under the exacting terms of discharge and recharge, can also make
With 10 years with first-class high-energy-density and excellent security and long term life characteristic.
Although caused with knowing that dendrite (dendrite) is formed as the negative pole of secondary cell using lithium metal in the past
Battery short circuit and the blast for thus causing danger, structural and electrical property can be maintained, can reach again reversible lithium from
Son insertion (intercalation) and the carbons compound for departing from just replace the lithium metal.
Relative to standard hydrogen electrode current potential, the carbons compound has the low-down discharge potential of about -3V, and because of stone
The very reversible discharge and recharge that the uniaxial orientation of black alkene layer (graphene layer) causes runs and shows excellent electricity
Pole life characteristic.Also, when Li ion chargings, electrode potential is 0VLi/Li+, can show almost with pure lithium metal phase
As current potential, therefore, with when with oxide-based positive pole constitute battery when, the advantage of energy higher can be obtained.
The secondary battery cathode is prepared as follows, i.e. using as the carbon material of negative electrode active material 13, with
And conductive material as needed and binder phase mixing are come after preparing a kind of negative electrode active material slurry, in monolayer fashion
By the slurry coating in the electrode collector 11 of Copper Foil etc, and it is dried.Now, when the slurry is applied, in order that
Active material powder is crimped on collector so that thickness uniformizing, implementation calendering procedure (reference picture 1) of electrode.
But, in the past when the calendering procedure of electrode is carried out, compared with the inside of negative electrode active material, surface by buckling
Must aggravate, so as to reduce hole (pore) ratio on surface.
The thickness of electrode is thicker, and this phenomenon is more obvious, also, as electrolyte is difficult to be impregnated into the inside of electrode and nothing
Method ensures the mobile path of ion, so as to be difficult to swimmingly realize the movement of ion, therefore, battery performance and life-span can be caused special
The reduction of property.
The content of the invention
Technical problem
Problem to be solved by this invention is to include multilayer active material layer by negative pole, is thus provided to electrode
The negative pole that internal ion mobility is improved.
Also, the present invention is also provided, it is improved by charge characteristic and life characteristic comprising the negative pole, battery
Lithium secondary battery.
Technical scheme
In order to solve described problem, the negative pole that an embodiment of the invention is provided, including：
Electrode collector；Negative electrode active material layer, comprising the multilayer active matter being formed on the electrode collector
Matter layer, and the multilayer active material layer includes the first negative electrode active material；And secondary negative electrode active material layer, comprising relative
The second negative electrode active with relatively low compacted density and larger average particle size for first negative electrode active material
Material.
Also, an embodiment of the invention, there is provided the lithium secondary battery comprising the negative pole.
Beneficial effect
The negative pole of one embodiment of the invention, by electrode collector include containing negative electrode active material compacted density and
The multilayer active material layer of two kinds of different negative electrode active materials of average particle size, so as to can also be improved after calendering procedure
The porosity (porosity) of electrode surface, and mobility of the ion to electrode interior can be improved, therefore, it is possible to usefully be applicable
In lithium secondary battery, and the charge characteristic and life characteristic of lithium secondary battery can be improved.
Brief description of the drawings
Fig. 1 is the ideograph of the conventional negative pole structure being made up of monolayer active material layer.
Fig. 2 is the ideograph of the negative pole structure being made up of multilayer active material layer of one embodiment of the invention.
Fig. 3 is the figure of the charge characteristic of the lithium secondary battery that embodiment 1 and comparative example 1 and 2 are determined according to experimental example 2
Table.
Fig. 4 and Fig. 5 are the lithium secondary battery that embodiment 1 and comparative example 1 based on negative pole density are determined according to experimental example 3
The chart of life characteristic.
The explanation of reference
11、21：Electrode collector
13：Negative electrode active material
23：First negative electrode active material
24：Second negative electrode active material
A：Negative electrode active material layer
B：Secondary negative electrode active material layer
Specific embodiment
Hereinafter, the present invention is described in detail.
The negative pole of one embodiment of the invention, as shown in the ideograph of Fig. 2, it may include：Electrode collector 21；One time negative pole is lived
Property material layer A, including the multilayer active material layer on the electrode collector is formed at, and the multilayer active material layer is included
First negative electrode active material 23；And secondary negative electrode active material layer B, comprising tool for relatively described first negative electrode active material
There is the second negative electrode active material 24 of relatively low compacted density and larger average particle size.
The negative pole of one embodiment of the invention, by electrode collector include containing negative electrode active material compacted density and
The multilayer active material layer of two kinds of different negative electrode active materials of average particle size, so as to can also be improved after calendering procedure
The porosity of electrode surface, and mobility of the ion to electrode interior can be improved, therefore, it is possible to improve the charging of lithium secondary battery
Characteristic and life characteristic.
First, the electrode collector, can be selected from by stainless steel, aluminium, nickel, titanium, calcining carbon, copper, by carbon, nickel, titanium
Or silver be surface-treated stainless steel, aluminium-cadmium alloy, the nonconductive polymers being surface-treated by conductive material and lead
Conductive polymers composition group in one or two.
Also, in negative pole of the invention, as first negative electrode active material and the second negative electrode active material, can
To enumerate theoretic greatest limit capacity as the crystallization of the native graphite and Delanium etc of 372mAh/g (844mAh/cc)
The noncrystalline class carbon or their mixture of matter class carbon, soft carbon (soft carbon) and hard carbon (hard carbon) etc, with
Just it is able to ensure that high-energy-density.
Specifically, first negative electrode active material and the second negative electrode active material, both can be respectively spherical in shape or class
The crystal class carbon of spheroidal same (of the same race) native graphite and Delanium etc, or other.
Also, in the negative pole of one embodiment of the invention, first negative electrode active material and the second negative electrode active material
The ratio between average particle size of matter can be 1:9 to 5:5.1, more specifically, can be 1:1.3 to 1:4.As nonrestrictive
One, the average particle size of first negative electrode active material can be about less than 20 μm, specifically, can be at such as 10 μm
To 18 μm of scope.
For example, the average particle size of the negative electrode active material of one embodiment of the invention, using laser diffractometry
(laser diffraction method) is measured.Generally, the laser diffractometry is from sub-micron (submicron) scope
Start, the particle diameter of number mm or so can be determined, and the result of high reproducibility and high de-agglomeration can be obtained.Negative electrode active material
Average particle size D50The particle diameter in 50% benchmark of particle diameter distribution can be defined as.
Also, in the negative pole of one embodiment of the invention, first negative electrode active material and the second negative electrode active material
The ratio between compacted density of matter is 1.1 under the pressure condition of 12 to 16MPa:1 to 3:1, preferably 1.1:1 to 1.5:1.
An embodiment of the invention, the compacting of first negative electrode active material and the second negative electrode active material is close
Degree, as long as disclosure satisfy that the first negative electrode active material of above range and the compacted density ratio of the second negative electrode active material, just not
It is particularly limited.But preferably, for example, the compacted density of the first negative electrode active material under the pressure of 12 to 16MPa for 1.4 to
1.85g/cc, the compacted density of the second negative electrode active material is 1.4 to 1.6g/cc under the pressure of 12 to 16MPa.
The compacted density is that the comparing that the degree of particle deformation is carried out occurs to negative electrode active material, when with identical
When pressure is rolled, compacted density value is lower, and compressive strength is more excellent.To first negative electrode active material and the second negative pole
The measure of the compacted density of active material, can be used the powder electricity of such as Mitsubishi Chemical (Mitsubishi chemical) company
Resistance measuring instrument MCP-PD51 is measured.In the case of using the powder resistance measuring instrument, in the pressure measurement unit of cylinder type
The negative electrode active material powder of ormal weight is put into part (load cell), and continues pressure, now, determine particle depressed
When density.The intensity of particle is bigger, will not more be pressed at the same pressure, therefore, by percent consolidation can present it is relatively low.
Also, in the negative pole of one embodiment of the invention, first negative electrode active material and the second negative electrode active material
The ratio between compressive strength can be 2 under the pressure condition of 12 to 16MPa:8 to 5:5.1, specifically, can be 2:8 to 4:7
Scope.
Also, the porosity of the whole volume of a negative electrode active material layer, for example, comprising 0.1 to 10 μm of size
The ratio of hole be for about 10 to 50 percentage by weights, and in the whole volume of the secondary negative electrode active material layer, hole
Rate is for about 10 to 50 percentage by weights.Now, compared with the pore size and/or porosity of negative electrode active material layer, two
Pore size and/or porosity in secondary negative electrode active material layer can relatively large or height.For example, in a negative electrode active material layer
And the porosity of secondary negative electrode active material layer is similarly in the case of 27%, the active matter of a negative electrode active material layer
The size of the hole between matter and active material can be 0.4 to 3 μm, the active material and activity of secondary negative electrode active material layer
Pore size between material can be 0.5 to 3.5 μm.
That is, negative pole of the invention, in the way of forming secondary negative electrode active material layer on a negative electrode active material layer
Improve the porosity on the surface of negative electrode active material layer such that it is able to prevent the negative electrode active material layer when calendering procedure is carried out
Surface damage, and the pore structure of electrode interior can be improved, wherein, a negative electrode active material layer is relative by compacted density
Higher than the first negative electrode active material that the second negative electrode active material and average particle size are relatively shorter than the second negative electrode active material
Composition, the secondary negative electrode active material layer is by compacted density is relatively low and average particle size is relatively large the second negative electrode active
Material composition.
On the other hand, in the case where the conventional electrode being made up of monolayer active material layer is formed, due to calendering procedure
Shi Yin softer (soft) and the characteristic of the weak single negative electrode active material layer of stress, it is impossible to pressure is transmitted to the inside of electrode,
Therefore, the negative electrode active material only positioned at the surface of electrode is subject to severe crush.For example, such as above-mentioned second negative electrode active material
Matter, in the case where the big monolayer active material layer of the low and average particle size merely with compacted density forms electrode, also due to
The characteristic of stress weak single negative electrode active material layer during calendering procedure so that only positioned at the negative electrode active material on the surface of electrode
Matter is subject to severe crush.As a result, because the porosity between the negative electrode active material of the near surface of electrode is reduced, thus to
The ion mobility reduction of electrode interior.The thickness of electrode of negative pole is thicker or density is higher, and this phenomenon may be more serious.
But, such as the present invention, if using high two or more of stress because compacted density and average particle size are different
Negative electrode active material, be especially relatively lower than a negative electrode active material layer using the compacted density of secondary negative electrode active material layer
Negative electrode active material, then the compressive strength for being coated on the negative electrode active material of the near surface of electrode is more excellent, during calendering
The pressing phenomenon of electrode surface is got over and can be relaxed.Therefore, with the inside of electrode, i.e. compared with a negative electrode active material layer,
The surface of electrode, i.e. the porosity of secondary negative electrode active material layer can be higher, therefore, be conducive to ion to be moved to electrode interior,
So as to improve ion mobility (reference picture 2).
First negative electrode active material of the invention and the second negative electrode active material, as needed, moreover it is possible to comprising conductive material
And binding agent.
Now, the conductive material, can illustrate nickel by powder, cobalt oxide, titanium oxide and carbon etc..As carbon, can enumerate
Selected from a certain kind in the group being made up of Ketjen black, acetylene black, furnace black, graphite, carbon fiber and fullerene or two kinds in them
Mixture above etc..
Also, the binding agent, it is possible to use all resin glues of lithium secondary battery are used in the past, as
Example, by selected from a certain kind in the group being made up of Kynoar, carboxymethylcellulose calcium, methylcellulose and Sodium Polyacrylate or
Two or more mixture in them etc..
Also, an embodiment of the invention, there is provided the preparation method of negative pole, the preparation method of the negative pole includes：
The step of first negative electrode active material slurry of the coating comprising the first negative electrode active material and resin glue on electrode collector
Suddenly；A step of negative electrode active material layer being formed in the way of drying the first negative electrode active material slurry；Described one
Second negative electrode active material slurry of the coating comprising the second negative electrode active material and resin glue on secondary negative electrode active material layer
The step of；The step of secondary negative electrode active material layer being formed in the way of drying the second negative electrode active material slurry；And
The step of electrode collector to being formed with a negative electrode active material layer and secondary negative electrode active material layer rolls.
Also, the above method can apply the second negative electrode active material before the first negative electrode active material slurry is dried
Slurry.That is, the step of applying the first negative electrode active material slurry and the second negative electrode active material slurry can be in no drying
The step of being carried out continuously in the case of step, also, coated slurry is dried, is rolled also can disposably be realized.
The calendering procedure can be performed under with conventional electrode preparation method identical process conditions.
In the method for the invention, before the calendering procedure is carried out, the inside of a negative electrode active material layer
Pore size be for about 1 to 20 μm, the porosity in a whole volume for negative electrode active material layer is for about 50%.But,
Carry out after calendering procedure, the pore size of an inside for negative electrode active material layer is for about 0.1 to 3 μm, a negative electrode active
Porosity in the whole volume of material layer is for about 10% to about 50%.
Also, before the calendering procedure is carried out, the pore size of the inside of the secondary negative electrode active material layer is
About 1 to 30 μm, the porosity in the whole volume of secondary negative electrode active material layer is for about 50%.But, carrying out calendering procedure
Afterwards, the pore size of the inside of secondary negative electrode active material layer is for about 0.1 to 5 μm, in the whole of secondary negative electrode active material layer
Porosity in individual volume is for about 10% to 50%.
In a negative electrode active material layer and secondary negative electrode active material layer, the ratio between porosity before calendering can be
5:5.1, the ratio between porosity after calendering can be 5:5.1 to 2:8.
Also, the pore size and/or porosity in secondary negative electrode active material layer can be with relatively large or higher than once bearing
The pore size and/or porosity of pole active material layer, for example, in a negative electrode active material layer and secondary negative electrode active material
The ratio between porosity of layer is 4:6 (20%:30%) in the case of, the size of the hole of a negative electrode active material layer can be with
It it is 0.4 to 3 μm, the pore size of secondary negative electrode active material layer can be 0.5 to 3.5 μm.
Generally, in the negative pole for being applicable negative electrode active material, the hole of 0.1 to 10 μm of size plays the leaching for improving electrolyte
The effect of the transmission speed of stain speed and lithium ion.If using the negative pole being only made up of monolayer active material layer as in the past,
Then after calendering procedure is carried out, the porosity on negative pole, for example, more than 5 μm of hole ratio is reduced to less than 50%, makes close
Degree is improved.
The measure of above-mentioned porosity is not particularly limited, can an embodiment of the invention, for example, by wish bright Nore-
Emmett-Taylor (BET, Brunauer-Emmett-Teller) determination method or mercury impregnating method (Hg porosimeter) are surveyed
It is fixed.
In the present invention, there is provided by utilizing compacted density and the mutually different two kinds of negative electrode active materials of average particle size
Multilayer active material layer composition negative pole, so as to after calendering procedure, the porosity on the top of negative pole is relatively higher than negative pole
Bottom porosity, thus make the density step-down on the top of negative pole.Therefore, it is possible to make electrolyte easily be soaked to electrode interior
Stain, can also improve ion mobility.And then, when the calendering procedure for later electrode preparation is carried out, can also maintain electrode
The surface form of active material that will not easily crush or be pressed.
Also, the present invention is provided and enclosed in outside battery by conventional method with by the negative pole, positive pole, dividing plate and electrolyte
Lithium secondary battery prepared by the mode of shell.
The positive pole, as long as the common positive pole used when lithium secondary battery is prepared, is just not particularly limited, example
Such as, can be by the slurry coating of mixed cathode active material powder, binding agent and conductive material is in electrode collector and is done
After dry, shaped by rolling.
The positive active material, it is preferable that be selected from by LiMn2O4、LiCoO2、LiNiO2、LiFeO2And V2O5Group
Into group in a certain kind or two or more mixture in them etc..Furthermore it is preferred that using TiS, MoS, organic disulfide
Compound compound or organic polysulfide compounds etc. can make the material that lithium is adsorbed and departed from.
As above-mentioned binding agent, Kynoar, carboxymethylcellulose calcium, methylcellulose and Sodium Polyacrylate can be enumerated
Deng as above-mentioned conductive material, the electric conductivity auxiliary material such as acetylene black, furnace black, graphite, carbon fiber and fullerene can be enumerated.
Also, used as dividing plate, as long as lithium secondary battery can be used in, any material can be used, for example, can
To include polyethylene, polypropylene or their multilayer film, Kynoar, polyamide and glass fibre etc..
As the electrolyte of lithium secondary battery, lithium salts can be included and be dissolved in the organic electrolyte of non-aqueous solvent or poly-
Polymer electrolyte.
As the non-aqueous solvent for constituting above-mentioned organic electrolyte, propene carbonate, ethylene carbonate, carbon can be included
Sour butene esters, benzonitrile, acetonitrile, tetrahydrofuran, 2- methyltetrahydrofurans, gamma-butyrolacton, dioxolanes, 4- methyl dioxy penta
Ring, N,N-dimethylformamide, dimethylacetylamide, dimethyl sulfoxide (DMSO), dioxanes, 1,2- dimethoxy-ethanes, sulfolane, two
Chloroethanes, chlorobenzene, nitrobenzene, dimethyl carbonate, methyl ethyl carbonate, diethyl carbonate, methyl propyl carbonate, carbonic acid first isopropyl ester,
The non-aqueous solvents such as ethyl butyl carbonate, dipropyl carbonate, diisopropyl carbonate, dibutyl carbonate, diethylene glycol (DEG) and dimethyl ether are mixed
The two or more mixed solvent in these solvents is closed, or, it is especially, excellent as material known to secondary lithium batteries solvent
Selection of land, a middle mixed carbonic acid dimethyl ester, methyl ethyl carbonate in propene carbonate, ethylene carbonate and butylene and
One in diethyl carbonate.
As the lithium salts, can be used and be selected from LiCl, LiBr, LiI, LiClO4、LiBF4、LiB10Cl10、LiPF6、
LiCF3SO3、LiCF3CO2、LiAsF6、LiSbF6、LiAlCl4、CH3SO3Li、CF3SO3Li、(CF3SO2)2It is NLi, chloroborane lithium, low
One or more lithium salts in level aliphatic carboxylic acid lithium and 4- phenylboric acid lithiums.
The polyelectrolyte, can include above-mentioned organic electrolyte and moisten comprising roc in above-mentioned organic electrolyte
The excellent PEO of property, PPOX, poly- acetonitrile, Kynoar, polymethacrylates and polymethylacrylic acid
The material of the copolymers such as methyl esters.
Secondary cell of the invention is due to the security and stabilization that play high-energy-density, high power characteristic, be improved
Property, it is the structure battery of big-and-middle-sized battery module so as to enable in particular to preferably use.Therefore, the present invention is also provided includes as above institute
The secondary cell stated as unit cells big-and-middle-sized battery module.
This big-and-middle-sized battery module can be preferably applied to the needs such as electric automobile, hybrid vehicle and electrical storage device
The power source of high power, Large Copacity.
Hereinafter, embodiments of the invention and comparative example are recorded.But, following examples are to a currently preferred implementation
The record of example, the present invention will not be restricted because of following embodiments.
For the mode for carrying out an invention
(embodiment 1)
It is the first negative electrode active material (artificial stone of 1.79g/cc to mix the negative pole density when the pressure of 12.3MPa is applied
Ink) 97.3 weight portions, conductive material (Super-P (conductive carbon black)) 0.7 weight portion, the weight of thickener (carboxymethylcellulose calcium) 1.0
Amount part and the weight portion of binding agent (butadiene-styrene rubber) 1.0, are thus prepared for the first negative electrode active material slurry.
Then, mixing negative pole density when the pressure of 12.3MPa is applied is the second negative electrode active material (people of 1.51g/cc
Make graphite) 97.3 weight portions, the weight portion of conductive material (Super-P) 0.7, the weight portion of thickener (carboxymethylcellulose calcium) 1.0 and
The weight portion of binding agent (butadiene-styrene rubber) 1.0, is thus prepared for the second negative electrode active material slurry.
Applied successively on copper collector above-mentioned first negative electrode active material slurry and the second negative electrode active material slurry it
Afterwards, it is dried, thus form the multilayer for being laminated once negative electrode active material layer and secondary negative electrode active material layer
Active material layer.
Then, the negative pole for forming above-mentioned multilayer active material layer is rolled using roll squeezer.Now, negative pole density
It is 1.6g/cc.Also, another negative pole that negative pole density is 1.64g/cc is obtained by identical method.
Then, positive active material (LiCoO is made2) 97.2 weight portions, the weight portion of binding agent (Kynoar) 1.5 and lead
The weight portion of electric material (Super-P) 1.3 is scattered in 1-METHYLPYRROLIDONE, is thus prepared for anode active material slurry.To
Above-mentioned slurry coating is rolled using roll squeezer afterwards on aluminium collector, so as to be prepared for positive pole (positive pole density：3.4g/
cc)。
It is put into polyethylene separator between above-mentioned negative pole and positive pole, and after putting it into battery case, injects electrolyte,
Thus it is prepared for secondary cell.Now, electrolyte uses the LiPF for being dissolved with 1.0M6Ethylene carbonate/methyl ethyl carbonate and
The mixed solution of diethyl carbonate (1/2/1 volume ratio), is thus prepared for secondary cell.
(comparative example 1)
It is the negative electrode active material (Delanium) of 1.51g/cc to mix the compacted density when the pressure of 12.3MPa is applied
97.3 weight portions, the weight portion of conductive material (Super-P) 0.7, the weight portion of thickener (carboxymethylcellulose calcium) 1.0 and binding agent
(butadiene-styrene rubber) 1.0 weight portion, is thus prepared for negative electrode active material slurry.
After above-mentioned negative electrode active material slurry is applied on the copper collector, it is dried, thus form individual layer
Active material layer.Afterwards, it is two kinds of 1.6g/cc and 1.64g/cc that negative pole density is prepared in the same manner as in Example 1
Negative pole and secondary cell.
(comparative example 2)
In addition to using negative electrode active material of the negative pole density as 1.78g/cc when being pressed with the strength of 12.3MPa,
To be prepared for negative pole density as the negative pole and secondary cell of 1.6g/cc with the identical method of comparative example 1.
(experimental example 1：The measure of compacted density meter average particle size)
To the measure of the compacted density of the particle of the negative electrode active material of preparation in embodiment 1, comparative example 1 and 2, three are used
The powder resistance measuring instrument MCP-PD51 of water chestnut chemical company is measured.
In the case of above-mentioned powder resistance measuring instrument, regulation is put into the load cell (load cell) of cylinder type
The positive electrode active material powder of amount, and continue pressure, now, density when measure particle is depressed.Therefore, negative electrode active material
The intensity of plasmid is bigger, and what is be pressed at the same pressure is fewer, so as to show relatively low density.Now, applied
Pressure shows about 12 to 16MPa or so.
The negative electrode active material of preparation in embodiment 1, comparative example 1 and comparative example 2 is determined using laser diffractometry
Average particle size.
The compacted density meter average particle size of the particle that will be determined in the manner is shown in Table 1.
Table 1
(experimental example 2：Charge characteristic)
In order to evaluate the charge characteristic of the secondary cell prepared in above-described embodiment 1, comparative example 1 and comparative example 2,23
The secondary cell that will be prepared in embodiment 1, comparative example and comparative example 2 under the conditions of DEG C is at constant current/constant voltage (CC/CV)
Under the conditions of 4.2V, 0.05C are charged to the condition of 0.1C after, be discharged to the condition of 0.1C under the conditions of constant current (CC)
3V, and determine capacity twice.Afterwards, charged to the condition of 0.5C under the conditions of constant current/constant voltage (CC/CV)
After 4.2V, 0.05C, 3V is discharged to the condition of 0.2C under the conditions of constant current (CC), determines the charging of 0.5C- multiplying powers
Characteristic.In the results are shown in Fig. 3.
That is, Fig. 3 is observed, if the rated current of charging 0.5C- multiplying powers (rate), with comparative example 1 and the battery of comparative example 2
Compare, it is more long that constant current charge time of the battery of embodiment 1 is presented.Therefore, it can confirm and have to include that individual layer is lived
The comparative example 1 of negative pole and the battery of comparative example 2 of property material layer are compared, the implementation with the negative pole including multilayer active material layer
The charge characteristic of the battery of example 1 is more excellent.
(experimental example 3：Life characteristic)
After being performed with the condition of above-mentioned experimental example 2, with 0.2C's under the conditions of constant current/constant voltage (CC/CV)
Condition charges to 4.2V, 0.05C, afterwards under the conditions of constant current (CC), is discharged to 3V with the condition of 0.2C, and implement repeatedly
80 circulations.In Fig. 4 and Fig. 5 is shown in this life characteristic result.
Now, the negative pole density that Fig. 4 presents embodiment 1, comparative example 1 and comparative example 2 is the secondary cell of 1.6g/cc
Life characteristic, Fig. 5 presents the negative pole density of embodiment 1 and comparative example 1 for the life-span of the secondary cell of 1.64g/cc is special
Property.
First, observation Fig. 4 is it has been confirmed that when negative pole density is down to 1.6g/cc, with including monolayer active material layer
The battery of the comparative example 1 of negative pole and the battery of comparative example 2 and the embodiment 1 with the negative pole including multilayer active material layer is equal
The life characteristic of similar level is presented.
But, Fig. 5 is it has been confirmed that when negative pole density increases to 1.64g/cc for observation, with being lived including multilayer negative pole
In the case of the electrode of the embodiment 1 of the electrode of property material layer, even if negative pole density is high, negative pole life characteristic is also very excellent, phase
Instead, in the case of the battery of the comparative example 1 with the electrode including individual layer negative electrode active material layer, if negative pole density is high,
Life characteristic reduction.
Therefore, it is known that the electrode of the embodiment 1 of the electrode with the multilayer active material layer including being obtained from the present invention
Compared with the electrode of comparative example 1, ion mobility is improved, therefore, speed and cycle characteristics are improved.
Claims (14)
1. a kind of negative pole, including：
Electrode collector；With
The multilayer active material layer on above-mentioned electrode collector is formed at,
Wherein above-mentioned multilayer active material layer is included：
An anode active material layer comprising the first negative electrode active material；With
Secondary negative electrode active material layer comprising the second negative electrode active material, second negative electrode active material relatively described first
There is relatively low compacted density and larger average particle size for negative electrode active material,
Wherein described first negative electrode active material and the second negative electrode active material include crystalline class carbon respectively.
2. negative pole according to claim 1, wherein first negative electrode active material and the second negative electrode active material difference
Comprising the spheroidal native graphite of spherical in shape or class, Delanium or their mixture.
3. negative pole according to claim 1, wherein first negative electrode active material and the second negative electrode active material is flat
The ratio between equal particle size is 1:9 to 5:5.1.
4. negative pole according to claim 1, wherein first negative electrode active material and the second negative electrode active material is flat
The ratio between equal particle size is 1:1.3 to 1:4.
5. negative pole according to claim 1, wherein the pressure of first negative electrode active material and the second negative electrode active material
The ratio between real density is 1.1 under the pressure condition of 12MPa to 16MPa:1 to 3:1.
6. negative pole according to claim 1, wherein the pressure of first negative electrode active material and the second negative electrode active material
Contracting intensity ratio is 2 under the pressure condition of 12MPa to 16MPa:8 to 5:5.1.
7. negative pole according to claim 1, wherein the porosity of the secondary negative electrode active material layer more than it is described once
The porosity of negative electrode active material layer.
8. negative pole according to claim 1, wherein the once negative electrode active material layer and secondary negative electrode active material layer
Conductive material and binding agent are also included respectively.
9. a kind of method for preparing negative pole, methods described includes：
First negative electrode active material slurry of the coating comprising the first negative electrode active material and resin glue on electrode collector
The step of；
A step of negative electrode active material layer is formed by drying the first negative electrode active material slurry；
Second negative pole of the coating comprising the second negative electrode active material and resin glue on a negative electrode active material layer
The step of active material slurry；
The step of secondary negative electrode active material layer is formed by drying the second negative electrode active material slurry；And
What the electrode collector to being formed with a negative electrode active material layer and secondary negative electrode active material layer was rolled
Step,
Wherein described first negative electrode active material and the second negative electrode active material include crystalline class carbon respectively.
10. a kind of method for preparing negative pole, methods described includes：
First negative electrode active material slurry of the coating comprising the first negative electrode active material and resin glue on electrode collector
The step of；
Coating comprising the second negative electrode active material and resin glue second is negative on the first negative electrode active material slurry
The step of pole active material slurry；
Multilayer negative electrode active is formed by drying the first negative electrode active material slurry and the second negative electrode active material slurry
The step of material layer；And
The step of electrode collector to being formed with the multilayer negative electrode active material layer rolls,
Wherein described multilayer negative electrode active material layer includes a negative electrode active material layer and secondary negative electrode active material layer,
Wherein described first negative electrode active material and the second negative electrode active material include crystalline class carbon respectively.
11. method according to claim 9 or 10, wherein the porosity of the secondary negative electrode active material layer relatively larger than
The porosity of negative electrode active material layer.
12. methods according to claim 11, wherein the once negative electrode active material layer and secondary negative electrode active material
The ratio between porosity before the calendering of layer is 5:5.1 to 4:6.
13. methods according to claim 11, wherein the once negative electrode active material layer and secondary negative electrode active material
The ratio between porosity after the calendering of layer is 5:5.1 to 2:8.
A kind of 14. lithium secondary batteries, its negative pole for including claim 1.
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| KR20130008785 | 2013-01-25 | ||
| KR10-2013-0008785 | 2013-01-25 | ||
| KR10-2014-0007308 | 2014-01-21 | ||
| KR1020140007308A KR101560471B1 (en) | 2013-01-25 | 2014-01-21 | Anode for lithium secondary battery and lithium secondary battery comprising the same |
| CN201480000767.2A CN104126242A (en) | 2013-01-25 | 2014-01-22 | Anode for lithium secondary battery and lithium secondary battery including same |
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| CN201480000767.2A Division CN104126242A (en) | 2013-01-25 | 2014-01-22 | Anode for lithium secondary battery and lithium secondary battery including same |
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| KR101560471B1 (en) | 2015-10-15 |
| CN104126242A (en) | 2014-10-29 |
| KR20140095980A (en) | 2014-08-04 |
| JP6120382B2 (en) | 2017-04-26 |
| CN106935793B (en) | 2020-02-14 |
| JP2015511389A (en) | 2015-04-16 |
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