CN112979875B - 一种聚合物电解质及其制备方法与应用 - Google Patents
一种聚合物电解质及其制备方法与应用 Download PDFInfo
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- CN112979875B CN112979875B CN202110182200.3A CN202110182200A CN112979875B CN 112979875 B CN112979875 B CN 112979875B CN 202110182200 A CN202110182200 A CN 202110182200A CN 112979875 B CN112979875 B CN 112979875B
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- polymer electrolyte
- lithium
- battery
- polymer
- sodium
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- 239000005518 polymer electrolyte Substances 0.000 title claims abstract description 155
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 54
- 239000011159 matrix material Substances 0.000 claims abstract description 39
- 239000000178 monomer Substances 0.000 claims abstract description 38
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 24
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 24
- 239000010452 phosphate Substances 0.000 claims abstract description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 21
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 claims abstract description 17
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 claims abstract description 15
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 5
- 239000003792 electrolyte Substances 0.000 claims description 74
- 229910052744 lithium Inorganic materials 0.000 claims description 46
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 32
- 239000012528 membrane Substances 0.000 claims description 31
- 239000011734 sodium Substances 0.000 claims description 28
- -1 lithium hexafluorophosphate Chemical group 0.000 claims description 27
- 239000003999 initiator Substances 0.000 claims description 25
- 159000000000 sodium salts Chemical class 0.000 claims description 25
- 239000004014 plasticizer Substances 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 20
- 229910052708 sodium Inorganic materials 0.000 claims description 19
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 18
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 18
- 238000011065 in-situ storage Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 17
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 229910003002 lithium salt Inorganic materials 0.000 claims description 10
- 159000000002 lithium salts Chemical class 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 9
- 125000003118 aryl group Chemical group 0.000 claims description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- ZMVMBTZRIMAUPN-UHFFFAOYSA-H [Na+].[V+5].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O Chemical compound [Na+].[V+5].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZMVMBTZRIMAUPN-UHFFFAOYSA-H 0.000 claims description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000004080 punching Methods 0.000 claims description 6
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004760 aramid Substances 0.000 claims description 4
- 229920003235 aromatic polyamide Polymers 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 4
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 4
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 claims description 4
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 3
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 3
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- 229920001651 Cyanoacrylate Polymers 0.000 claims description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 3
- MWCLLHOVUTZFKS-UHFFFAOYSA-N Methyl cyanoacrylate Chemical compound COC(=O)C(=C)C#N MWCLLHOVUTZFKS-UHFFFAOYSA-N 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 3
- 125000004386 diacrylate group Chemical group 0.000 claims description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 125000003709 fluoroalkyl group Chemical group 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- ZTOMUSMDRMJOTH-UHFFFAOYSA-N glutaronitrile Chemical compound N#CCCCC#N ZTOMUSMDRMJOTH-UHFFFAOYSA-N 0.000 claims description 3
- 125000001072 heteroaryl group Chemical group 0.000 claims description 3
- DEUISMFZZMAAOJ-UHFFFAOYSA-N lithium dihydrogen borate oxalic acid Chemical compound B([O-])(O)O.C(C(=O)O)(=O)O.C(C(=O)O)(=O)O.[Li+] DEUISMFZZMAAOJ-UHFFFAOYSA-N 0.000 claims description 3
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 3
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 3
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 claims description 3
- MCVFFRWZNYZUIJ-UHFFFAOYSA-M lithium;trifluoromethanesulfonate Chemical compound [Li+].[O-]S(=O)(=O)C(F)(F)F MCVFFRWZNYZUIJ-UHFFFAOYSA-M 0.000 claims description 3
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 229940047670 sodium acrylate Drugs 0.000 claims description 3
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical group [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 claims description 3
- 229910001488 sodium perchlorate Inorganic materials 0.000 claims description 3
- 229910001495 sodium tetrafluoroborate Inorganic materials 0.000 claims description 3
- XGPOMXSYOKFBHS-UHFFFAOYSA-M sodium;trifluoromethanesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C(F)(F)F XGPOMXSYOKFBHS-UHFFFAOYSA-M 0.000 claims description 3
- IAHFWCOBPZCAEA-UHFFFAOYSA-N succinonitrile Chemical compound N#CCCC#N IAHFWCOBPZCAEA-UHFFFAOYSA-N 0.000 claims description 3
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- NDZWKTKXYOWZML-UHFFFAOYSA-N trilithium;difluoro oxalate;borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-].FOC(=O)C(=O)OF NDZWKTKXYOWZML-UHFFFAOYSA-N 0.000 claims description 3
- OXFUXNFMHFCELM-UHFFFAOYSA-N tripropan-2-yl phosphate Chemical compound CC(C)OP(=O)(OC(C)C)OC(C)C OXFUXNFMHFCELM-UHFFFAOYSA-N 0.000 claims description 3
- QLCATRCPAOPBOP-UHFFFAOYSA-N tris(1,1,1,3,3,3-hexafluoropropan-2-yl) phosphate Chemical compound FC(F)(F)C(C(F)(F)F)OP(=O)(OC(C(F)(F)F)C(F)(F)F)OC(C(F)(F)F)C(F)(F)F QLCATRCPAOPBOP-UHFFFAOYSA-N 0.000 claims description 3
- ZMQDTYVODWKHNT-UHFFFAOYSA-N tris(2,2,2-trifluoroethyl) phosphate Chemical compound FC(F)(F)COP(=O)(OCC(F)(F)F)OCC(F)(F)F ZMQDTYVODWKHNT-UHFFFAOYSA-N 0.000 claims description 3
- 241001474374 Blennius Species 0.000 claims description 2
- XSAOIFHNXYIRGG-UHFFFAOYSA-M lithium;prop-2-enoate Chemical compound [Li+].[O-]C(=O)C=C XSAOIFHNXYIRGG-UHFFFAOYSA-M 0.000 claims description 2
- 238000007790 scraping Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000004132 cross linking Methods 0.000 abstract description 28
- 238000006243 chemical reaction Methods 0.000 abstract description 22
- 229920001187 thermosetting polymer Polymers 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 239000004634 thermosetting polymer Substances 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 20
- 238000001125 extrusion Methods 0.000 description 15
- 238000002485 combustion reaction Methods 0.000 description 14
- 238000004880 explosion Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- 238000002474 experimental method Methods 0.000 description 13
- 238000009472 formulation Methods 0.000 description 13
- 239000002994 raw material Substances 0.000 description 13
- 230000014759 maintenance of location Effects 0.000 description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical group [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 11
- 229910001416 lithium ion Inorganic materials 0.000 description 11
- 229910052786 argon Inorganic materials 0.000 description 10
- 239000010405 anode material Substances 0.000 description 9
- 239000010406 cathode material Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 229920000388 Polyphosphate Polymers 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000007773 negative electrode material Substances 0.000 description 6
- 239000001205 polyphosphate Substances 0.000 description 6
- 235000011176 polyphosphates Nutrition 0.000 description 6
- 239000007774 positive electrode material Substances 0.000 description 5
- 239000007784 solid electrolyte Substances 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 4
- 229910000733 Li alloy Inorganic materials 0.000 description 4
- 229940048053 acrylate Drugs 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001989 lithium alloy Substances 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000011149 active material Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000011244 liquid electrolyte Substances 0.000 description 3
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229920006254 polymer film Polymers 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- IKULXUCKGDPJMZ-UHFFFAOYSA-N sodium manganese(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Na+] IKULXUCKGDPJMZ-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- CWPKTBMRVATCBL-UHFFFAOYSA-N 3-[1-[1-[(2-methylphenyl)methyl]piperidin-4-yl]piperidin-4-yl]-1h-benzimidazol-2-one Chemical compound CC1=CC=CC=C1CN1CCC(N2CCC(CC2)N2C(NC3=CC=CC=C32)=O)CC1 CWPKTBMRVATCBL-UHFFFAOYSA-N 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- 229910002984 Li7La3Zr2O12 Inorganic materials 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- DWYMPOCYEZONEA-UHFFFAOYSA-L fluoridophosphate Chemical compound [O-]P([O-])(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-L 0.000 description 2
- 238000010574 gas phase reaction Methods 0.000 description 2
- 229910021385 hard carbon Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
- FRMOHNDAXZZWQI-UHFFFAOYSA-N lithium manganese(2+) nickel(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Ni+2].[Li+] FRMOHNDAXZZWQI-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 1
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical group NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
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- BDKWOJYFHXPPPT-UHFFFAOYSA-N lithium dioxido(dioxo)manganese nickel(2+) Chemical compound [Mn](=O)(=O)([O-])[O-].[Ni+2].[Li+] BDKWOJYFHXPPPT-UHFFFAOYSA-N 0.000 description 1
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- 238000005457 optimization Methods 0.000 description 1
- 150000005677 organic carbonates Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
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- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
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- YPPMLCHGJUMYPZ-UHFFFAOYSA-L sodium;iron(2+);sulfate Chemical compound [Na+].[Fe+2].[O-]S([O-])(=O)=O YPPMLCHGJUMYPZ-UHFFFAOYSA-L 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- VPOIXCYASUPXIC-UHFFFAOYSA-J tetrasodium oxalate Chemical compound C(C(=O)[O-])(=O)[O-].C(C(=O)[O-])(=O)[O-].[Na+].[Na+].[Na+].[Na+] VPOIXCYASUPXIC-UHFFFAOYSA-J 0.000 description 1
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Images
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Abstract
本发明公开一种聚合物电解质及其制备方法与应用,其中,所述聚合物电解质包括聚合物基质,所述聚合物基质为由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体自聚形成的聚合物,或为由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体与其他单体共聚形成的聚合物。所述聚合物电解质可用于电池中,所述聚合物基质可以在130~190℃的高温条件下发生自交联反应,生成致密的热固性高分子可以切断离子传输,防止电池热失控的发生;并且该自交联反应为吸热反应,有助于快速降低电池温度,阻止电池热失控;所述聚合物电解质还可以捕获自由基,具有本征阻燃性;该聚合物基质的以上特征协同作用,可以有效防止电池热失控的发生。
Description
技术领域
本发明涉及电池电解质技术领域,特别涉及一种聚合物电解质及其制备方法与应用。
背景技术
二次锂离子电池具有高能量密度、长循环寿命、无记忆效应等优点,目前已广泛应用于3C电子产品、电动汽车等领域。然而,目前商业化的锂电池常用易挥发、易燃的有机碳酸酯类液态电解液,易导致起火、爆炸等安全隐患。为了提高电池的安全性,研究人员提出了一系列优化措施,包括改变电解液溶剂、设计高浓盐电解液以及使用无机固态电解质或聚合物电解质等。其中,使用聚合物电解质代替液态电解液是一种行之有效的方法。相对于目前商业化的碳酸酯类电解液,聚合物电解质具有机械强度高、电极-电解质界面相容性好以及安全性高等优势,具有巨大的实际应用潜力。
目前文献报道了多种聚合物电解质体系,例如聚氧化乙烯(PEO)、聚甲基丙烯酸酯,聚碳酸酯等聚合物电解质体系。这些电解质体系,虽然展现了一定的应用潜力,但是电池的循环性能亟待提高。此外,虽然这些聚合物电解质没有电解液泄漏的风险,但并不能完全阻止电池热失控的发生,而且因其本征易燃性,在电池发生着火时会起到助燃作用。因此,发展具有高安全性聚合物电解质对高能量密度锂电池的实际应用具有重要的意义。
据报道,电池热失控的发生跟电极正、负极侧分别产生的氧气与可燃气(如氢气、乙烷等)的气相反应息息相关,而常规阻燃性电解质(如磷酸酯类电解质)体系并不能阻止该反应的发生。电池热失控的发生往往始于电池负极侧SEI处电解液的不断分解导致的热累积,随后在不断热累积的情况下,负极SEI层分解暴露更多活性位点加剧电解液分解/PE隔膜融化造成电池内短路加剧电池升温,进而电池正极的活性材料(~200℃)发生分解产生大量的氧气,与产生的可燃气(如负极产生的氢气、乙烷等)/液体电解液溶剂发生剧烈反应,最终导致电池热失控的发生。本征阻燃的聚合物电解质由于在高温下不具有切断该气相反应的能力,因此并不能阻止电池热失控的发生。因此,发展具有高温二次交联导致电池自关闭能力的聚合物电解质是实现高能量密度锂电池高安全性的关键。聚磷酸酯基电解质因其阻燃性,受到科学家们的广泛关注。目前,多篇专利公开了聚磷酸酯基电解质体系。如上所述,虽然这些聚磷酸酯基电解质具有阻燃性,但仍然不能完全避免高能量密度锂电池在滥用条件(如短路、挤压、针刺等)下热失控的发生。例如,CN107863555B和CN107819151B分别公开了一种不燃性的含有聚磷酸酯聚合物的固态电解质和复合型固态电解质,但该聚合物电解质不具有高温下二次交联的能力,因此难以降低高能锂电池(如NCM811/Li金属电池)在针刺和挤压条件下因短路造成的热失控风险;CN107819156B公开了一种通过低分子量端环氧基甲基膦酸酯齐聚物、锂盐和电池添加剂的电解液前体溶液原位固化制备的不燃性聚合物电解质,然而该电解质具有低室温离子电导率(1.3×10-4~4.5×10-4Scm-1)和窄的电位窗口(4~5V),难以满足高能量密度锂电池的需求。而且,这种通过原位端环氧基开环聚合制备聚合物电解质的方法具有分子量低和单体转化率低的缺陷。再者,这种聚合物电解质虽然一定程度上提高了电池的阻燃性,但不具备高温下二次交联导致电池自关闭的能力;CN111499873A公开了一种聚磷酸基聚合物及其制备方法和应用。该聚合物基电解质虽然具有一定的阻燃性,但在高温下同样不具有高温二次交联导致电池自关闭的能力,因此也不能满足高比能锂电池安全性的要求;CN111620974A公开了一种用于高电压锂离子电池的含磷聚酯电解质,但其聚合物基质也不具有高温二次交联导致电池自关闭的反应性,故不能确保电池滥用条件下的安全性;CN110247111A和CN111253523A分别公开了可原位聚合的聚磷酸酯基聚合物电解质。这两种电解质虽然都具有不燃性和优异的电化学性质,但同样不具备高温下二次交联导致电池自关闭能力,因此也不能满足电池滥用条件下的安全性要求。
因此,开发具有高温自交联导致电池自关闭的高安全性聚磷酸酯基聚合物电解质对高比能锂电池的商业化应用具有重要的意义。
发明内容
鉴于上述现有技术的不足,本发明的目的在于提供一种高温自交联导致电池自关闭的高安全聚合物电解质及其制备方法与应用。
本发明的技术方案如下:
一种聚合物电解质,其中,其包括聚合物基质,所述聚合物基质为由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体自聚形成的聚合物,或为由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体与其他单体共聚形成的聚合物。
所述的聚合物电解质,其中,所述由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体为:
中的一种,其中,R1,R2,R3,R4,A,Y,Z分别独立地选自十八碳以下的烷基、氟代烷基、芳基或杂芳基中的一种;V取自H,甲基,F,CN或CF3中的一种;B选自O或NH;X-选自PF6 -,BF4 -,TFSI-或FSI-中的一种;m取值为0~8;U为C=O或O=S=O。
所述的聚合物电解质,其中,还包括锂或钠盐、塑化剂、引发剂和多孔支撑材料。
所述的聚合物电解质,其中,按质量百分比计包括10-85%的聚合物基质,0-29.9%的锂或钠盐,0-80%的塑化剂、0-1%的引发剂以及0-35%的多孔支撑材料。
所述的聚合物电解质,其中,所述锂盐为六氟磷酸锂、高氯酸锂、双草酸硼酸锂、二氟草酸硼酸锂、三氟甲磺酸锂、双三氟甲基磺酰亚胺锂、双氟磺酰亚胺锂和中的一种或多种,其中,R0取自十八碳以下的多氟代烷基、芳基;
和/或,所述塑化剂为二氧化硅,二氧化锆,二氧化钛,三氧化二铝,无机锂盐、无机钠盐、碳酸乙烯酯、碳酸二甲酯、碳酸甲乙酯、碳酸丙烯酯、碳酸二乙酯、丁二腈、戊二腈、氟代碳酸乙烯酯、三乙二醇二甲醚、环丁砜、磷酸三甲酯、磷酸三乙酯、磷酸三(2,2,2-三氟乙基)酯、磷酸三异丙酯和磷酸三(六氟异丙基)酯中的一种或多种;
和/或,所述多孔支撑材料为纤维素无纺膜、海藻纤维无纺膜、芳纶无纺膜、聚芳砜酰胺无纺膜、聚四氟乙烯无纺膜、聚丙烯无纺膜、玻璃纤维、聚对苯二甲酸乙二醇酯薄膜和聚酰亚胺无纺膜中的一种或多种;
和/或,所述引发剂为偶氮二异丁腈、偶氮二异庚腈、偶氮二异丁酸二甲酯、过氧化苯甲酰、过氧化苯甲酰叔丁酯和过氧化甲乙酮中的一种或多种。
所述的聚合物电解质,其中,所述聚合物基质为由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体与其他单体共聚形成的聚合物,所述其他单体为聚乙二醇单甲醚甲基丙烯酸酯、聚乙二醇二丙烯酸酯、甲基丙烯酸甲酯、丙烯腈、聚四氢呋喃二甲基丙烯酸酯、马来酸酐、醋酸乙烯酯、丙烯酰胺、氰基丙烯酸酯、丙烯酸锂、丙烯酸钠、 中的一种或多种,其中,B选自O或NH;V选自H,甲基;X-选自PF6 -,BF4 -,TFSI-或FSI-中的一种;n的取值为1-4的正整数。
所述的聚合物电解质,其中,所述聚合物基质中,按质量百分比计,其他单体占所述聚合物基质组分的0-95%,由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体占所述聚合物基质组分的5-100%。
一种聚合物电解质的制备方法,其中,包括步骤:
将聚合物基质、锂或钠盐、塑化剂和引发剂混合,通过原位聚合反应,生成所述聚合物电解质;
或者,将聚合物基质、锂或钠盐和塑化剂分散在溶剂中,然后刮涂至多孔支撑材料上,烘干制得所述聚合物电解质;
或者,将聚合物基质和塑化剂分散在溶剂中,然后刮涂至多孔支撑材料上,经过干冲片后吸收由塑化剂和锂或钠盐组成的电解液,制得所述聚合物电解质。
所述聚合物电解质的制备方法,其中,所述溶剂为二甲基亚砜、N-甲基吡咯烷酮、N,N-二甲基甲酰胺、1,4-二氧六环、乙二醇二甲醚、氯仿、二氯甲烷和乙酸乙酯中的一种或多种。
一种聚合物电解质的应用,其中,将本发明所述的聚合物电解质用于制备电池。
有益效果:与现有技术相比,本发明提供的聚合物电解质不仅热尺寸稳定性好,在高温下不易变形可避免造成电池界面破坏或内短路,而且能在通常发生电池热失控的高温条件(130~190℃)下进一步交联聚合生成热固性高分子,阻断电荷传输,防止电池短路,使电池温度无法继续上升,从而避免电池热失控的发生;另外,该自交联反应为吸热反应,而且反应迅速,有助于快速降低电池温度,阻止电池热失控;而且,生成的热固性高分子可以捕获自由基,具有本征阻燃性;该聚合物电解质的以上特征协同作用,可以有效防止电池热失控的发生。
本发明提供的聚合物电解质可以在正极、负极/电解质界面成膜,能稳定电极/电解质界面的稳定性;具有宽的电化学窗口,能匹配高电压正极,提高电池的能量密度;所述聚合物电解质的机械强度高,可以稳定电极结构和抑制枝晶;其含有氨基甲酸酯片段,可以在电解质中形成氢键网络,使电解质具有高自修复性能。
本发明获得的聚合物电解质制备简单,电化学性能优异,并能够有效确保电池的安全性能。所述电解质可应用到高能量密度的锂金属电池、锂合金负极电池、钠金属电池、锂/钠-硫电池以及其他二次电池(如钾金属电池、锌电池、非水系镁电池等)中。
附图说明
图1为由实施例1中聚合物电解质组装的电池在室温和50℃的长循环性能对比图。
图2为由实施例1中聚合物电解质组装的电池在热处理前后的阻抗变化结果图。
图3为由实施例2中聚合物电解质组装的电池在室温时的长循环性能结果图。
图4为由实施例2中聚合物电解质组装的电池在热处理前后的阻抗变化结果图。
图5为由实施例3中聚合物电解质组装的电池在50℃下的长循环性能结果图。
图6为由实施例3中聚合物电解质组装的电池在热处理前后的阻抗变化结果图。
图7为由实施例4中聚合物电解质组装的电池在室温时的长循环性能结果图。
图8为由实施例12中聚合物电解质组装的电池在室温时的长循环性能结果图。
具体实施方式
本发明提供一种聚合物电解质及其制备方法与应用,为使本发明的目的、技术方案及效果更加清楚、明确,以下对本发明进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
本发明提供了一种聚合物电解质,其包括聚合物基质,所述聚合物基质为由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体自聚形成的聚合物,或为由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体与其他单体共聚形成的聚合物。
在本实施例中,所述聚合物电解质可用于电池中,所述聚合物基质可以在130~190℃的高温条件下发生自交联反应,生成致密的热固性高分子可以切断离子传输,防止电池热失控的发生;并且该自交联反应为吸热反应,而且反应迅速,有助于快速降低电池温度,阻止电池热失控;进一步,所述聚合物电解质还可以捕获自由基,具有本征阻燃性;该聚合物基质的以上特征协同作用,可以有效防止电池热失控的发生。
在一些实施方式中,所述由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体为:
中的一种,其中,R1,R2,R3,R4,A,Y,Z分别独立地选自十八碳以下的烷基、氟代烷基、芳基或杂芳基中的一种;V取自H,甲基,F,CN或CF3中的一种;B选自O或NH;X-选自PF6 -,BF4 -,TFSI-或FSI-中的一种;m取值为0~8;U为C=O或O=S=O。
在本实施例中,所述聚合物电解质的应用与电池的高安全性主要源于聚合物基质中氨基甲酸酯基团与磷酸酯基团在130~190℃的高温条件下发生的自交联吸热反应以及本征阻燃性协同作用来实现的。
在一些实施方式中,所述聚合物电解质,还包括锂或钠盐、塑化剂、引发剂和多孔支撑材料。
在一些具体的实施方式中,所述聚合物电解质按质量百分比计包括10-85%的聚合物基质,0-29.9%的锂或钠盐,0-80%的塑化剂、0-1%的引发剂以及0-35%的多孔支撑材料。
按本实施例配比制得的聚合物电解质,其氧化分解电压>5.0V(vs.Li/Li+),室温离子电导率为0.2~5.5×10-3S/cm,拉伸强度为0.5~60MPa。
在一些具体的实施方式中,所述锂盐为六氟磷酸锂、高氯酸锂、双草酸硼酸锂、二氟草酸硼酸锂、三氟甲磺酸锂、双三氟甲基磺酰亚胺锂、双氟磺酰亚胺锂和中的一种或多种,但不限于此,其中,R0取自十八碳以下的多氟代烷基、芳基;
在一些具体的实施方式中,所述钠盐为高氯酸钠、磷酸钒钠、三氟甲磺酸钠、六氟磷酸钠、双草酸硼酸钠、二氟草酸硼酸钠、三氟甲磺酰亚胺钠、四氟硼酸盐钠和中的一种或多种,但不限于此,其中,R0取自十八碳以下的多氟代烷基、芳基。
在一些具体的实施方式中,所述塑化剂为二氧化硅,二氧化锆,二氧化钛,三氧化二铝,无机锂盐、无机钠盐、碳酸乙烯酯、碳酸二甲酯、碳酸甲乙酯、碳酸丙烯酯、碳酸二乙酯、丁二腈、戊二腈、氟代碳酸乙烯酯、三乙二醇二甲醚、环丁砜、磷酸三甲酯、磷酸三乙酯、磷酸三(2,2,2-三氟乙基)酯、磷酸三异丙酯和磷酸三(六氟异丙基)酯中的一种或多种,但不限于此;其中,无机锂盐为Li3aLa(2/3)-aTiO3(0.04<a<0.14)、Li3+bEaQ1-bO4(E=Si、Sc、Ge、Ti;Q=P、As、V、Cr,0<b<1)、LiZr2(PO4)3、Li7La3Zr2O12、Li1+cAlcTi2-c(PO4)3(0<c<2)、Li1+ dAldGe2-d(PO4)3(0<d<2)、Li3OCl、Li3OCl0.5Br0.5、Li10GeP2S12、Li14Zn(GeO4)4、Li5La3Z2O12(Z=Ta、Nb)、Li5.5La3Nb1.75In0.25O12、Li3N-LiU(U=Cl、Br、I)、Li9-neDeN2Cl3(D=Na、K、Rb、Cs、Mg、Al,0<e<9,0<n<4)、3Li3N-JI(J=Li、Na、K)、LiPON、Li2S-LfSg(L=Al、Si、P,0<f<3,0<g<6)、Li6PS5I(I=F,Cl,Br,I);将所述无机锂盐中的锂替换成钠,得到相应的无机钠盐。
在一些具体的实施方式中,所述多孔支撑材料为纤维素无纺膜、海藻纤维无纺膜、芳纶无纺膜、聚芳砜酰胺无纺膜、聚四氟乙烯无纺膜、聚丙烯无纺膜、玻璃纤维、聚对苯二甲酸乙二醇酯薄膜和聚酰亚胺无纺膜中的一种或多种,但不限于此。
在一些具体的实施方式中,所述引发剂为偶氮二异丁腈(AIBN)、偶氮二异庚腈(ABVN)、偶氮二异丁酸二甲酯(AIBME)、过氧化苯甲酰(BPO)、过氧化苯甲酰叔丁酯(TBPB)、过氧化甲乙酮(MEKPO)的一种或多种,但不限于此。
在一些实施方式中,所述聚合物基质为由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体与其他单体共聚形成的聚合物,所述其他单体为聚乙二醇单甲醚甲基丙烯酸酯、聚乙二醇二丙烯酸酯、甲基丙烯酸甲酯、丙烯腈、聚四氢呋喃二甲基丙烯酸酯、马来酸酐、醋酸乙烯酯、丙烯酰胺、氰基丙烯酸酯、丙烯酸锂、丙烯酸钠、 中的一种或多种,其中,B选自O或NH;V选自H,甲基;X-选自PF6 -,BF4 -,TFSI-或FSI-中的一种;n的取值为1-4的正整数。优选地,所述其他单体为丙烯腈、甲基丙烯酸甲酯或中的一种。
在一些具体的实施方式中,所述聚合物基质中,按质量百分比计,其他单体占所述聚合物基质组分的0-95%,由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体占所述聚合物基质组分的5-100%。
在一些具体的实施方式中,所述聚合物基质中,锂盐为六氟磷酸锂,钠盐为三氟甲磺酰亚胺钠,塑化剂为二氧化硅或磷酸三甲酯,多孔支撑材料为纤维素或芳纶无纺膜,引发剂为偶氮二异丁腈。
在一些实施方式中,还提供一种聚合物电解质的制备方法,其包括步骤:
将聚合物基质、锂或钠盐、塑化剂和引发剂混合,通过原位聚合反应,生成所述聚合物电解质。
本实施例是采用原位聚合法来制备聚合物电解质的,其具体可包括以下步骤:将锂或钠盐以一定的比例与塑化剂(或无机颗粒)混合均匀,得到混合物;向所述混合物中加入由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体或由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体/其他单体、以及引发剂得到均一的前驱体溶液;将上述前驱体溶液注入含有正负极的锂/钠电池中,在40℃~80℃条件下,使基于丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体自聚或基于丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体与其他单体原位共聚合,得到高温自交联导致电池自关闭的高安全聚合物电解质。
在一些实施方式中,还提供另一种聚合物电解质的制备方法,其包括步骤:将聚合物基质、锂或钠盐和塑化剂分散在溶剂中,然后刮涂至多孔支撑材料或四氟乙烯板上,烘干制得所述聚合物电解质;或者,将聚合物基质和塑化剂分散在溶剂中,然后刮涂至多孔支撑材料或四氟乙烯板上,经过干冲片后吸收由塑化剂和锂或钠盐组成的电解液,制得所述聚合物电解质。
本实施例采用非原位聚合法来制备所述聚合物电解质,所述溶剂为二甲基亚砜、N-甲基吡咯烷酮、N,N-二甲基甲酰胺、1,4-二氧六环、乙二醇二甲醚、氯仿、二氯甲烷和乙酸乙酯中的一种或多种,但不限于此。本实施例提供的聚合物电解质的制备方法简单,其电化学性能优异,并能够有效确保电池的安全性能。所述电解质可应用到高能量密度的锂金属电池、锂合金负极电池、钠金属电池、锂/钠-硫电池以及其他二次电池(如钾金属电池、锌电池、非水系镁电池等)中。
在一些实施方式中,还提供一种聚合物电解质的应用,将本发明所述的聚合物电解质用于制备电池。所述电池可以为高能量密度的锂金属电池、锂合金负极电池、钠金属电池、锂/钠-硫电池以及其他二次电池,所述二次电池可以为钾金属电池、锌电池、非水系镁电池等。
在本实施例中,所述聚合物电解质可以在正极、负极/电解质界面成膜,能稳定电极/电解质界面的稳定性;具有宽的电化学窗口,能匹配高电压正极,提高电池的能量密度;所述聚合物电解质的机械强度高,可以稳定电极结构和抑制枝晶;其含有氨基甲酸酯片段,可以在电解质中形成氢键网络,使电解质具有高自修复性能。
在一些具体的实施方式中,所述电池包括正极、负极以及介于所述正极和所述负极之间的聚合物电解质。所述正极的活性材料为钴酸锂、磷酸铁锂、磷酸锰铁锂、锰酸锂、镍锰酸锂、富锂锰基、三元材料、锂离子氟磷酸盐、锂钒氟磷酸盐、锂铁氟磷酸盐、锂锰氧化物,或NaxPR(CN)6(P,R为Fe,Co,Ni,Mn)、磷酸钒钠,硫、硫酸铁钠,钠离子氟磷酸盐,钠钒氟磷酸盐,钠铁氟磷酸盐,钠锰氧化物,钠钴氧化物或共轭有机化合物中的一种。所述负极的活性材料为金属锂、金属锂合金、金属钠、金属钠合金、钛酸钠、硬碳、石墨、二硫化钼、钛酸锂、石墨烯、氧化锑、硅、硅碳和硅薄膜中的一种。
下面通过具体实施例对本发明一种聚合物电解质及其制备方法做进一步的解释说明:
实施例1
用于制备该聚合物电解质的原料配比如表1所示,在充满氩气的手套箱中配置LiTFSI/EMC溶液。将和丙烯腈加入上述溶液中,并加入引发剂AIBN,完全溶解后,将溶液注入含有正、负极材料的锂离子电池中,放置在60℃条件下使其原位聚合,8h后得到所需要的聚合物电解质电池。
表1:
由上述实施例1所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表1)。将上述获得电解质组装NCM622/Li金属全电池,在运行电压2.5~4.4V和0.1C下分别在室温和50℃下循环100圈后容量保持率分别为90%和87%(如图1所示),可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的NCM622/锂金属电池在180℃处理30s,测试表明电池界面阻抗增高了超过50倍(如图2所示),表明该聚合物电解质可以在180℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例2
用于制备该聚合物电解质的原料配比如表2所示。将按表2所示单体比例预先制备的聚氨酯丙烯酸酯溶解于NMP中,混合均匀后刮涂至PET上,经烘干得聚合物膜。将该聚合物膜冲片后,在溶液中充分溶胀,得聚合物电解质膜。将该电解质膜与相应的正、负极材料组装锂电池。
表2:
由上述实施例2所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表2)。将上述电解质组装NCM811/锂金属全电池,在运行电压2.5~4.3V和2.0C下循环100圈后容量保持率为89%(如图3所示),可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的NCM811/锂金属电池在150℃处理50s,测试表明电池界面阻抗增高了超过10倍(如图4所示),表明该聚合物电解质可以在150℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例3
用于制备该聚合物电解质的原料配比如表3所示,在充满氩气的手套箱中,将碳酸亚乙烯酯和LiDFOB共同混合配成溶液,并加入引发剂BPO,完全溶解后,将溶液注入含有正负极材料的锂离子电池中,放置在80℃条件下使其原位聚合,6h后得到所需要的聚合物电解质电池。
表3:
由上述实施例3所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表3)。将上述电解质组装钴酸锂/石墨全电池,在工作电压2.5~4.4V和0.5C下在50℃循环200圈后容量保持率为91%(如图5所示),可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的NCM811/锂金属电池在165℃处理20s,测试表明电池界面阻抗增高了约10倍(如图6所示),表明该聚合物电解质可以在165℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例4
用于制备该聚合物电解质的原料配比如表4所示,在充满氩气的手套箱中配置溶液,搅拌均匀备用。将 加入到上述溶液中,再加入引发剂ABVN,完全溶解后,将溶液注入含有正、负极材料的锂离子电池中,放置在70℃条件下使其原位聚合,8h后得到所需要的聚合物电解质电池。
表4:
由上述实施例4所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表4)。将上述获得电解质组装NCM811/Si-C600全电池,在工作电压2.5~4.5V和0.1C下循环400圈后容量保持率为89%(如图7所示),可见所得聚合物电解质具有优异的电化学性能。
经测试表明,该聚合物电解质可以在130度发生自交联反应。将上述聚合物电解质组装的NCM811/Si-C600全电池在130度处理1min,测试表明电池界面阻抗增高超过30倍,说明电池实现了自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例5
用于制备该聚合物电解质的原料配比如表5所示,在充满氩气的手套箱中,将和聚乙二醇丙烯酸酯以及Li7La3Zr2O12混合均匀中,再加入引发剂AIBN,完全溶解后,将溶液注入含有正负极材料的锂离子电池中,放置在40℃条件下使其原位聚合,10h后得到所需要的聚合物电解质电池。
表5:
由上述实施例5所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表5)。将上述电解质组装硫/Li电池,在工作电压1.0~3.0V和0.5C下循环300圈后剩余容量为1000mAh/g,可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的锂硫电池在145℃处理20s,测试表明电池界面阻抗增高了约40倍,表明该聚合物电解质可以在145℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例6
用于制备该聚合物电解质的原料配比如表6所示,在充满氩气的手套箱中配置LiTFSI/四氢呋喃溶液,待其搅拌均匀备用。将溶解在上述溶液中,再加入引发剂AIBN,完全溶解后,将溶液注入含有正负极材料的锂离子电池中,放置在60℃条件下使其原位聚合,8h后得到所需要的聚合物电解质电池。
表6:
由上述实施例6所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表6)。将上述电解质组装钴酸锂/Si-C400全电池,在工作电压2.5~4.55V和0.1C下循环300圈后容量保持率为85%,可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的钴酸锂/Si-C400全电池在190℃处理15s,测试表明电池界面阻抗增高了约35倍,表明该聚合物电解质可以在190℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例7
用于制备该聚合物电解质的原料配比如表7所示,在充满氩气的手套箱中配置LiPF6/EC溶液,待其搅拌均匀备用。将和聚四氢呋喃二甲基丙烯酸酯加入上述溶液中,并加入TBPB,完全溶解后,将溶液注入含有正、负极材料的锂离子电池中,放置在60℃条件下使其原位聚合,6h后得到所需要的聚合物电解质电池。
表7:
由上述实施例7所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表7)。将上述电解质组装Li1.2Ni0.15Co0.1Mn0.55O2/Si全电池,在运行电压2.5~4.4V和0.1C下循环300圈后容量保持率为83%,可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的Li1.2Ni0.15Co0.1Mn0.55O2/Si全电池在185℃处理25s,测试表明电池界面阻抗增高了约45倍,表明该聚合物电解质可以在185℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例8
用于制备该聚合物电解质的原料配比如表8所示。在充满氩气的手套箱中将LiTFSI、SN、以及引发剂AIBME溶于无水DME中,混合均匀后刮涂至四氟乙烯板上,经烘干得电解质膜。将该电解质膜冲片后,与相应的正、负极材料组装锂电池。
将溶液注入含有正、负极材料的锂离子电池中,放置在60℃条件下使其原位聚合,12h后得到所需要的聚合物电解质电池。
表8:
由上述实施例8所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表8)。将该电解质组装镍锰酸锂/Si全电池,在工作电压2.5~5.0V和0.1C下循环120圈后容量保持率分别为90%,可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的镍锰酸锂/Si全电池全电池在180℃处理15s,测试表明电池界面阻抗增高了约40倍,表明该聚合物电解质可以在180℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例9
用于制备该电解质的原料配比如表9所示。将按表9所示单体比例预先制备的聚氨酯丙烯酸酯溶解于DMF溶剂中,混合均匀后刮涂至四氟乙烯板上,经烘干得聚合物膜。将聚合物膜冲片后,在DME-NaTFSI溶液中充分溶胀,得聚合物电解质膜。将该电解质膜与相应的正、负极材料组装锂电池。
将溶液注入含有正、负极材料的钠电池中,放置在60℃条件下使其原位聚合,12h后得到所需要的聚合物电解质电池。
由上述实施例9所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表9)。将上述获得电解质组装NaFeMn(CN)6/Na电池,在工作电压2.5~4.0V和0.2C下循环200圈后容量保持率分别为92%,可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的NaFeMn(CN)6/Na电池在140℃处理25s,测试表明电池界面阻抗增高了约40倍,表明该聚合物电解质可以在140℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例10
用于制备该电解质的原料配比如表10所示,在充满氩气的手套箱中配置NaTFSI/三乙二醇二甲醚溶液,然后加入 以及引发剂TPO,完全溶解后,将溶液注入含有正、负极材料的钠电池中,放置在60℃条件下使其原位聚合,12h后得到所需要的聚合物电解质电池。
由上述实施例10所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表9)。将上述获得电解质组装硫酸铁钠/石墨电池,在工作电压2.5~3.8V和0.1C下循环200圈后容量保持率分别为92%,可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的硫酸铁钠/Na电池在155℃处理25s,测试表明电池界面阻抗增高了约30倍,表明该聚合物电解质可以在155℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例11
用于制备该电解质的原料配比如表11所示,将预先制备的聚合物基质、钠盐、塑化剂在二甲基亚砜中混合均匀后刮涂至多孔支撑材料或四氟乙烯板上,经烘干得电解质膜。将该电解质膜冲片后,与相应的正、负极材料组装钠电池。
表11
由上述实施例所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表11)。将上述获得电解质组装钠锰氧化物/Na电池,在工作电压2.4~3.7V和0.5C下循环200圈后容量保持率分别为90%,可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的钠锰氧化物/硬碳电池在160℃处理25s,测试表明电池界面阻抗增高了约20倍,表明该聚合物电解质可以在160℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例12
用于制备该电解质的原料配比如表12所示,在充满氩气的手套箱中配置溶液,然后加入和醋酸乙烯酯以及引发剂TPO,完全溶解后,将溶液注入含有正、负极材料的钠电池中,放置在60℃条件下使其原位聚合,12h后得到所需要的聚合物电解质电池。
由上述实施例12所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表12)。将上述获得电解质组装磷酸钒钠/Na电池,在工作电压2.4~3.7V和0.1C下循环100圈后容量保持率分别为94%(如图8所示),可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的磷酸钒钠/Na电池在170℃处理20s,测试表明电池界面阻抗增高了约23倍,表明该聚合物电解质可以在170℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
实施例13
用于制备该电解质的原料配比如表13所示,在充满氩气的手套箱中配置溶液,然后加入和马来酸酐以及引发剂TPO,完全溶解后,将溶液注入含有正、负极材料的钠电池中,放置在60℃条件下使其原位聚合,12h后得到所需要的聚合物电解质电池。
由上述实施例13所得电解质具有高离子电导率、宽电化学窗口以及高的拉伸强度(表13)。将上述获得电解质组装S/Na电池,在工作电压1.5~2.8V和0.2C下循环200圈后容量保持率分别为80%,可见所得聚合物电解质具有优异的电化学性能。
将上述聚合物电解质组装的S/Na电池在160℃处理25s,测试表明电池界面阻抗增高了约25倍,表明该聚合物电解质可以在160℃下发生二次自交联反应,从而实现了电池的自关闭。该聚合物电解质电池经针刺和挤压实验,未发生燃烧和爆炸。
应当理解的是,本发明的应用不限于上述的举例,对本领域普通技术人员来说,可以根据上述说明加以改进或变换,所有这些改进和变换都应属于本发明所附权利要求的保护范围。
Claims (9)
2.根据权利要求1所述的聚合物电解质,其特征在于,还包括锂或钠盐、塑化剂、引发剂和多孔支撑材料。
3.根据权利要求1所述的聚合物电解质,其特征在于,按质量百分比计包括10-85%的聚合物基质,0-29.9%的锂或钠盐,0-80%的塑化剂、0-1%的引发剂以及0-35%的多孔支撑材料。
4.根据权利要求3所述的聚合物电解质,其特征在于,所述锂盐为六氟磷酸锂、高氯酸锂、双草酸硼酸锂、二氟草酸硼酸锂、三氟甲磺酸锂、双三氟甲基磺酰亚胺锂、双氟磺酰亚胺锂和中的一种或多种,其中,R0取自十八碳以下的多氟代烷基、芳基;
和/或,所述塑化剂为二氧化硅,二氧化锆,二氧化钛,三氧化二铝,无机锂盐、无机钠盐、碳酸乙烯酯、碳酸二甲酯、碳酸甲乙酯、碳酸丙烯酯、碳酸二乙酯、丁二腈、戊二腈、氟代碳酸乙烯酯、三乙二醇二甲醚、环丁砜、磷酸三甲酯、磷酸三乙酯、磷酸三(2,2,2-三氟乙基)酯、磷酸三异丙酯和磷酸三(六氟异丙基)酯中的一种或多种;
和/或,所述多孔支撑材料为纤维素无纺膜、海藻纤维无纺膜、芳纶无纺膜、聚芳砜酰胺无纺膜、聚四氟乙烯无纺膜、聚丙烯无纺膜、玻璃纤维、聚对苯二甲酸乙二醇酯薄膜和聚酰亚胺无纺膜中的一种或多种;
和/或,所述引发剂为偶氮二异丁腈、偶氮二异庚腈、偶氮二异丁酸二甲酯、过氧化苯甲酰、过氧化苯甲酰叔丁酯和过氧化甲乙酮中的一种或多种。
6.根据权利要求1所述的聚合物电解质,其特征在于,所述聚合物基质中,按质量百分比计,其他单体占所述聚合物基质组分的0-95%,由丙烯酰基、氨基甲酸酯和磷酸酯三个砌块共同组成的聚合单体占所述聚合物基质组分的5-100%。
7.一种如权利要求1-6任一所述聚合物电解质的制备方法,其特征在于,包括步骤:
将聚合物基质、锂或钠盐、塑化剂和引发剂混合,通过原位聚合反应,生成所述聚合物电解质;
或者,将聚合物基质、锂或钠盐和塑化剂分散在溶剂中,然后刮涂至多孔支撑材料上,烘干制得所述聚合物电解质;
或者,将聚合物基质和塑化剂分散在溶剂中,然后刮涂至多孔支撑材料上,经过干冲片后吸收由塑化剂和锂或钠盐组成的电解液,制得所述聚合物电解质。
8.根据权利要求7所述聚合物电解质的制备方法,其特征在于,所述溶剂为二甲基亚砜、N-甲基吡咯烷酮、N,N-二甲基甲酰胺、1,4-二氧六环、乙二醇二甲醚、氯仿、二氯甲烷和乙酸乙酯中的一种或多种。
9.一种聚合物电解质的应用,其特征在于,将权利要求1-6任一所述的聚合物电解质用于制备电池。
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