WO1999019917A2 - Composite suitable for use in electrochemical cells - Google Patents
Composite suitable for use in electrochemical cells Download PDFInfo
- Publication number
- WO1999019917A2 WO1999019917A2 PCT/EP1998/006394 EP9806394W WO9919917A2 WO 1999019917 A2 WO1999019917 A2 WO 1999019917A2 EP 9806394 W EP9806394 W EP 9806394W WO 9919917 A2 WO9919917 A2 WO 9919917A2
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- WIPO (PCT)
- Prior art keywords
- layer
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- weight
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- composite
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 239000000203 mixture Substances 0.000 claims abstract description 93
- 150000001875 compounds Chemical class 0.000 claims abstract description 87
- 239000007787 solid Substances 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000003475 lamination Methods 0.000 claims abstract description 16
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims abstract description 15
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- 238000006116 polymerization reaction Methods 0.000 claims abstract description 14
- 230000009471 action Effects 0.000 claims abstract description 12
- 229920000570 polyether Polymers 0.000 claims abstract description 12
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 11
- 238000003851 corona treatment Methods 0.000 claims abstract description 9
- 125000000524 functional group Chemical group 0.000 claims abstract description 8
- 239000011164 primary particle Substances 0.000 claims abstract description 8
- 239000007859 condensation product Substances 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 24
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- 238000005304 joining Methods 0.000 claims description 8
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- 238000002844 melting Methods 0.000 claims description 6
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- -1 lithium cations Chemical class 0.000 description 85
- 239000000243 solution Substances 0.000 description 30
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 15
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- QDWJJTJNXAKQKD-UHFFFAOYSA-N trihexyphenidyl hydrochloride Chemical compound Cl.C1CCCCC1C(C=1C=CC=CC=1)(O)CCN1CCCCC1 QDWJJTJNXAKQKD-UHFFFAOYSA-N 0.000 description 6
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- 229910052782 aluminium Inorganic materials 0.000 description 4
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- 125000003118 aryl group Chemical group 0.000 description 4
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- 125000003438 dodecyl group Chemical group [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])* 0.000 description 4
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- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
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- 229940052303 ethers for general anesthesia Drugs 0.000 description 1
- HUNISAHOCCASGM-UHFFFAOYSA-N ethyl 2-dimethoxyphosphorylacetate Chemical compound CCOC(=O)CP(=O)(OC)OC HUNISAHOCCASGM-UHFFFAOYSA-N 0.000 description 1
- HJWBBBADPXPUPA-UHFFFAOYSA-N ethyl 3-(4-chlorophenyl)-5-methyl-1,2-oxazole-4-carboxylate Chemical compound CCOC(=O)C1=C(C)ON=C1C1=CC=C(Cl)C=C1 HJWBBBADPXPUPA-UHFFFAOYSA-N 0.000 description 1
- NOJFJZZMRDSOLM-UHFFFAOYSA-N ethyl diethoxyphosphorylformate Chemical compound CCOC(=O)P(=O)(OCC)OCC NOJFJZZMRDSOLM-UHFFFAOYSA-N 0.000 description 1
- 125000004428 fluoroalkoxy group Chemical group 0.000 description 1
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- 125000003976 glyceryl group Chemical group [H]C([*])([H])C(O[H])([H])C(O[H])([H])[H] 0.000 description 1
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- 125000000623 heterocyclic group Chemical group 0.000 description 1
- PYGSKMBEVAICCR-UHFFFAOYSA-N hexa-1,5-diene Chemical group C=CCCC=C PYGSKMBEVAICCR-UHFFFAOYSA-N 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 238000012690 ionic polymerization Methods 0.000 description 1
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- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
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- AFRJJFRNGGLMDW-UHFFFAOYSA-N lithium amide Chemical compound [Li+].[NH2-] AFRJJFRNGGLMDW-UHFFFAOYSA-N 0.000 description 1
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- 229910001540 lithium hexafluoroarsenate(V) Inorganic materials 0.000 description 1
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 description 1
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- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 229910001386 lithium phosphate Inorganic materials 0.000 description 1
- 229910001537 lithium tetrachloroaluminate Inorganic materials 0.000 description 1
- 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 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
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- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
- VHRYZQNGTZXDNX-UHFFFAOYSA-N methacryloyl chloride Chemical compound CC(=C)C(Cl)=O VHRYZQNGTZXDNX-UHFFFAOYSA-N 0.000 description 1
- CTSAXXHOGZNKJR-UHFFFAOYSA-N methyl 2-diethoxyphosphorylacetate Chemical compound CCOP(=O)(OCC)CC(=O)OC CTSAXXHOGZNKJR-UHFFFAOYSA-N 0.000 description 1
- SIGOIUCRXKUEIG-UHFFFAOYSA-N methyl 2-dimethoxyphosphorylacetate Chemical compound COC(=O)CP(=O)(OC)OC SIGOIUCRXKUEIG-UHFFFAOYSA-N 0.000 description 1
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- CZDSWLXAULJYPZ-UHFFFAOYSA-J molybdenum(4+);dicarbonate Chemical compound [Mo+4].[O-]C([O-])=O.[O-]C([O-])=O CZDSWLXAULJYPZ-UHFFFAOYSA-J 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- LSHROXHEILXKHM-UHFFFAOYSA-N n'-[2-[2-[2-(2-aminoethylamino)ethylamino]ethylamino]ethyl]ethane-1,2-diamine Chemical compound NCCNCCNCCNCCNCCN LSHROXHEILXKHM-UHFFFAOYSA-N 0.000 description 1
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- 230000007935 neutral effect Effects 0.000 description 1
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
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- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- UIUWNILCHFBLEQ-UHFFFAOYSA-N pent-3-enoic acid Chemical compound CC=CCC(O)=O UIUWNILCHFBLEQ-UHFFFAOYSA-N 0.000 description 1
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- ULSIYEODSMZIPX-UHFFFAOYSA-N phenylethanolamine Chemical compound NCC(O)C1=CC=CC=C1 ULSIYEODSMZIPX-UHFFFAOYSA-N 0.000 description 1
- 239000005054 phenyltrichlorosilane Substances 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
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- 229920002432 poly(vinyl methyl ether) polymer Polymers 0.000 description 1
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- 229920002480 polybenzimidazole Polymers 0.000 description 1
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- 229920000379 polypropylene carbonate Polymers 0.000 description 1
- 229920000346 polystyrene-polyisoprene block-polystyrene Polymers 0.000 description 1
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- 229910052700 potassium Inorganic materials 0.000 description 1
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- DNFFZVPOFBBNHH-UHFFFAOYSA-N prop-2-enyl 2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoate Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(=O)OCC=C DNFFZVPOFBBNHH-UHFFFAOYSA-N 0.000 description 1
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- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000004528 spin coating Methods 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
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- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
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- 125000004434 sulfur atom Chemical group 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
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- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052645 tectosilicate Inorganic materials 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- ISXOBTBCNRIIQO-UHFFFAOYSA-N tetrahydrothiophene 1-oxide Chemical compound O=S1CCCC1 ISXOBTBCNRIIQO-UHFFFAOYSA-N 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- FOZHTJJTSSSURD-UHFFFAOYSA-J titanium(4+);dicarbonate Chemical compound [Ti+4].[O-]C([O-])=O.[O-]C([O-])=O FOZHTJJTSSSURD-UHFFFAOYSA-J 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- GAJQCIFYLSXSEZ-UHFFFAOYSA-L tridecyl phosphate Chemical compound CCCCCCCCCCCCCOP([O-])([O-])=O GAJQCIFYLSXSEZ-UHFFFAOYSA-L 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- SFENPMLASUEABX-UHFFFAOYSA-N trihexyl phosphate Chemical compound CCCCCCOP(=O)(OCCCCCC)OCCCCCC SFENPMLASUEABX-UHFFFAOYSA-N 0.000 description 1
- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical class [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 description 1
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical class [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 description 1
- QJAVUVZBMMXBRO-UHFFFAOYSA-N tripentyl phosphate Chemical compound CCCCCOP(=O)(OCCCCC)OCCCCC QJAVUVZBMMXBRO-UHFFFAOYSA-N 0.000 description 1
- RXPQRKFMDQNODS-UHFFFAOYSA-N tripropyl phosphate Chemical compound CCCOP(=O)(OCCC)OCCC RXPQRKFMDQNODS-UHFFFAOYSA-N 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- WTLBZVNBAKMVDP-UHFFFAOYSA-N tris(2-butoxyethyl) phosphate Chemical compound CCCCOCCOP(=O)(OCCOCCCC)OCCOCCCC WTLBZVNBAKMVDP-UHFFFAOYSA-N 0.000 description 1
- QLNUSZCPEUTHBS-UHFFFAOYSA-N tris(2-methoxyethyl) phosphate Chemical compound COCCOP(=O)(OCCOC)OCCOC QLNUSZCPEUTHBS-UHFFFAOYSA-N 0.000 description 1
- DLEQRTPKFCPBDG-UHFFFAOYSA-N tris(oxolan-2-yl) phosphate Chemical compound C1CCOC1OP(OC1OCCC1)(=O)OC1CCCO1 DLEQRTPKFCPBDG-UHFFFAOYSA-N 0.000 description 1
- VOSUIKFOFHZNED-UHFFFAOYSA-N tris(prop-2-enyl) benzene-1,3,5-tricarboxylate Chemical compound C=CCOC(=O)C1=CC(C(=O)OCC=C)=CC(C(=O)OCC=C)=C1 VOSUIKFOFHZNED-UHFFFAOYSA-N 0.000 description 1
- NPXKBAHNVUNXSI-UHFFFAOYSA-N tris[2-(diethylamino)ethyl] phosphate Chemical compound CCN(CC)CCOP(=O)(OCCN(CC)CC)OCCN(CC)CC NPXKBAHNVUNXSI-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910009112 xH2O Inorganic materials 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 150000007934 α,β-unsaturated carboxylic acids Chemical class 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
-
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Definitions
- the present invention relates to composites which are suitable for, inter alia, electrochemical cells having electrolytes containing lithium ions; their use in, for example, electrodes; electrodes, sensors, electrochromic windows, displays, capacitors and ion-conducting films comprising such a composite; and also electrochemical cells which comprise such a molding.
- Electrochemical, in particular rechargeable, cells are generally known, for example from "Ullmann's Encyclopedia of Industrial Chemistry” , 5th Ed. , Vol. A3, VCH Verlagsgesellschaft mbH, Weinheim, 1985, pages 343-397.
- lithium batteries and lithium ion batteries in particular as secondary cells, owing to their high specific energy storage density.
- the cathode of such cells comprises lithiated manganese, cobalt, vanadium or nickel mixed oxides which in the stoichiometrically simplest case can be described as LiMn 2 0 4 , LiCo0 2 , iV 2 0 5 or LiNi0 2 .
- These mixed oxides react reversibly with compounds which can incorporate lithium ions into their lattice, for example graphite, with the lithium ions being removed from the crystal lattice and the metal ions such as manganese, cobalt or nickel ions present in the latter being oxidized.
- This reaction can be utilized in an electrochemical cell for storing electrical energy by separating the compound which takes up lithium ions, i.e. the anode material, and the lithium-containing mixed oxide, i.e. the cathode material, by means of an electrolyte through which the lithium ions migrate from the mixed oxide into the anode material (charging operation).
- the compounds suitable for the reversible storage of lithium ions are usually fixed on collector electrodes by means of a binder.
- a layer which is electrically insulating but permeable to lithium cations is located between the two electrodes.
- This layer can be a solid electrolyte or a conventional separator.
- the necessary battery films i.e. cathode, anode and separator films
- the cathode and anode film(s) are joined to collector electrodes in the form of, for example, an aluminum or copper foil.
- collector electrodes in the form of, for example, an aluminum or copper foil.
- the separator film has to withstand the mechanical stresses on its own, which presents no problem in the case of conventional separator films based on, for example, polyolefins and having the conventional thickness.
- JP 09-134 730 and JP 09-161 815 propose joining these separator films to the anode and/or cathode film by means of a bonding layer.
- This comprises at least one first layer which is filled with a solid, e.g. a separator layer, and at least one second layer which can be a cathode layer or an anode layer.
- the composite of the present invention thus comprises a separator layer/anode layer combination or separator layer/cathode layer combination or cathode layer/separator layer/anode layer combination; it is of course possible for further layers and/or support materials defined herein to be present.
- the present invention accordingly provides, in one embodiment, a composite comprising Aa) at least one first layer which comprises a mixture la, comprising a mix Ila consisting of
- the proportion by weight of the mix Ila in the mixture la is from 1 to 100% by weight, and the layer is free of an electron-conducting, electrochemically active compound,
- first layer or layers and the second layer or layers are joined to one another by one of the two methods VI or V2:
- V2 Corona treatment of the first layer or layers, the second layer or layers or the first layer or layers and the second layer or layers and subsequent bringing together of the corona-treated first layer or layers with the corona-treated or untreated second layer or layers.
- the first layer or layers preferably comprise(s) a mixture la comprising a mix Ha consisting of
- the present invention provides a composite comprising
- At least one first layer which comprises a mixture lb comprising a mix lib consisting of
- the layer is free of an electron-conducting, electrochemically active compound
- first layer or layers and the second layer or layers are joined to one another by one of the two methods VI or V2:
- V2 Corona treatment of the first layer or layers, the second layer or layers or the first layer or layers and the second layer or layers and subsequent bringing together of the corona-treated first layer or layers with the corona- treated second layer or layers.
- the present invention further provides a composite comprising at least one first layer Aa or at least one first layer Ab or at least one first layer Aa and at least one first layer Ab, at least one second layer B, each as defined above, and
- the solid III used in this layer is, first and foremost, an inorganic solid, preferably an inorganic basic solid, selected from the group consisting of oxides, mixed oxides, silicates, sulfates, carbonates, phosphates, nitrides, amides, imides and carbides of the elements of main groups I, II, III and IV and transition group IV of the Periodic Table; a polymer selected from the group consisting of polyethylene, polypropylene, polystyrene, polytetrafluoroethylene, polyvinylidene fluoride, polyamides, polyimides; a solids dispersion comprising such a polymer; and a mixture of two or more thereof.
- an inorganic solid preferably an inorganic basic solid, selected from the group consisting of oxides, mixed oxides, silicates, sulfates, carbonates, phosphates, nitrides, amides, imides and carbides of the elements of main groups I, II, III and IV and transition
- oxides such as calcium oxide, silicon dioxide, aluminum oxide, magnesium oxide or titanium dioxide, mixed oxides, for example of the elements silicon, calcium, aluminum, magnesium, titanium
- silicates such as ladder, chain, sheet and framework silicates, preferably wollastonite, in particular hydrophobicized wollastonite, sulfates such as alkali metal and alkaline earth metal sulfates; carbonates such as alkali metal and alkaline earth metal carbonates, e.g.
- phosphates such as apatites; nitrides; amides; imides; carbides; polymers such as polyethylene, polypropylene, polystyrene, polytetrafluoroethylene, polyvinylidene fluoride; polyamides; polyimides; or other thermoplastics, thermosets, microgels, solids dispersions, in particular those comprising the abovementioned polymers, and also mixtures of two or more of the abovementioned solids.
- inorganic solids which conduct Li ions preferably an inorganic basic solid which conducts Li ions, can be used according to the invention as solid III.
- lithium borates such as Li 4 B 6 O ⁇ * xH 2 O, Li 3 (B0 2 ) 3 , Li 9 B 4 O 7 * xH 2 0, LiB0 2 , where x can be from 0 to 20; lithium aluminates such as Li 2 0 * A1 2 0 3 * H 2 0, Li 2 Al 2 0 4 , LiA10 2 ; lithium aluminosilicates such as lithium-containing zeolites, feldspars, feldspar substitutes, phyllosilicates and inosilicates, and, in particular, LiAlSi 2 O 6 (spodumene),
- LiAlSi 4 O 10 (petullite), LiAlSi0 4 (eucryptite), mica such as K[Li,Al] 3 [AlSi] 4 O 10 (F-OH) 2 ,/ K[Li,Al,Fe] 3 [AlSi] 4 O 10 (F-OH) 2 ; lithium zeolites, in particular those in fiber, sheet or cube form, in particular those having the formula Li 2/z O * Al 2 O 3 * xSi0 2 * yH 2 0, where z corresponds to the valence, x is from 1.8 to about 12 and y is from 0 to about 8; lithium carbides such as Li 2 C 2 , Li 4 C; Li 3 N; lithium oxides and mixed oxides such as LiA10 2 , Li 2 Mn0 3 , Li 2 0, Li 2 0 2 , Li 2 Mn0 4 , Li 2 Ti0 3 ; Li 2 NH; LiNH 2 ; lithium phosphates such as Li 3 P0 4
- Particularly suitable solids III are basic solids.
- basic solids are those whose mixture with a liquid, water- containing diluent which itself has a pH of at most 7 has a higher pH than this diluent.
- the solids are preferably very largely insoluble in the liquid used as electrolyte and electrochemically inert in the battery medium.
- Particularly suitable solids are those which have a primary particle size of from 5 nm to 20 ⁇ m, preferably from 0.01 to 10 ⁇ m and in particular from 0.1 to 5 ⁇ m, where the particle sizes specified are determined by electron microscopy.
- the melting point of the solid is preferably above the operating temperature customary for the electrochemical cell; melting points of above 120°C, in particular above 150° C, have been found to be particularly useful.
- the solids can be symmetrical, i.e. have an aspect ratio height: width: length of about 1 and be in the form of spheres, granules, approximately round structures, but also in the form of any polyhedra such as cuboids, tetrahedra, hexahedra, octahedra or bipyramids, or can be distorted or asymmetric, i.e. have an aspect ratio height: width: length different from 1 and be in the form of needles, asymmetric tetrahedra, asymmetric bipyramids, asymmetric hexahedra or octahedra, platelets, disks or as fibers. If the solids are in the form of asymmetric particles, the abovementioned upper limit for the primary particle size relates in each case to the smallest axis.
- the compound VI is preferably selected from the group consisting of monohydric or polyhydric alcohols having only carbon atoms in the main chain; monohydric or polyhydric alcohols whose main chain comprises at least two carbon atoms plus at least one atom selected from the group consisting of oxygen, phosphorus and nitrogen; silicon-containing compounds; amines having at least one primary amino group; amines having at least one secondary amino group; aminoalcohols; monohydric or polyhydric thiols; compounds containing at least one thiol group and at least one hydroxyl group; and mixtures of two or more thereof.
- preferred compounds are: monohydric or polyhydric alcohols which have only carbon atoms in the main chain and have from 1 to 20, preferably from 2 to 20 and in particular from 2 to 10, alcoholic OH groups, in particular dihydric, trihydric and tetrahydric alcohols, preferably having from 2 to 20 carbon atoms, e.g.
- ethylene glycol 1,2- or 1,3-propanediol, 1,2- or 1,3-butanediol, 1,4-butenediol or 1,4-butynediol, 1,6-hexanediol, neopentyl glycol, 1,2- dodecanediol, glycerol, trimethylolpropane, pentaerythritol or sugar alcohols, hydroquinone, novolak, bisphenol A; it is also possible, as can be seen from the above definition, to use monohydric alcohols such as methanol, ethanol, propanol, n-, sec- or tert-butyl, etc.; use can also be made of polyhydroxyolefins, preferably those having two terminal hydroxyl groups, e.g.
- polyester polyols as are known, for example, from Ullmanns Encyclopadie der ischen Chemie, 4th edition, Volume 19, pp. 62-65 and are obtained, for example, by reaction of dihydric alcohols with polybasic, preferably dibasic, polycarboxylic acids; monohydric or polyhydric alcohols whose main chain comprises at least two carbon atoms plus at least one oxygen atom, preferably polyether alcohols such as polymerization products of alkylene epoxides, for example isobutylene oxide, propylene oxide, ethylene oxide, 1,2-epoxybutane, 1,2- epoxypentane, 1,2-epoxyhexane, tetrahydrofuran, styrene oxide; use can also be made of polyether alcohols which are modified at the end groups, e.g.
- polyether alcohols modified by NH 2 end groups these alcohols preferably have a molecular weight (number average) of from 100 to 5000, more preferably from 200 to 1000 and in particular from 300 to 800; such compounds are known per se and are commercially available, for example under the trade names Pluriol or Pluronic (BASF Aktiengesellschaft); alcohols as defined above in which some or all carbon atoms are replaced by silicon; compounds of this type which can be used are, in particular, polys iloxanes or alkylene oxide-siloxane copolymers or mixtures of polyether alcohols and polysiloxanes as are described, for example, in EP-B 581 296 and EP-A 525 728; as regards the molecular weight of these alcohols, what has been said above also applies; alcohols as defined above, in particular polyether alcohols, in which some or all oxygen atoms are replaced by sulfur atoms; with regard to the molecular weight of these alcohols, what has been said above likewise applies; monohydric or polyhydric alcohol
- lactones which are derived from compounds of the formula HO-(CH 2 ) z - COOH, where z is from 1 to 20, e.g. e-caprolactone, j ⁇ -propiolactone, 7-butyrolactone or methyl-e-caprolactone; silicon-containing compounds such as dichlorosilane or trichlorosilane, phenyltrichlorosilane, diphenyldichlorosilane, dimethylvinylchlorosilane; silanols such as trimethylsilanol; amines having at least one primary and/or secondary amino group, e.g.
- aliphatic thiols such as methane thiol, ethanethiol, cyclohexanethiol, dodecanethiol; aromatic thiols such as thiophenol, 4-chlorothiophenol, 2-mercaptoaniline; compounds containing at least one thiol group and at least one hydroxyl group, e.g.
- amino alcohols such as ethanolamine, N-methylethanolamine, N-ethylethanolamine, N-butylethanolamine, 2-amino-l-propanol, 2-amino-l- phenylethanol, monoamino or polyamino polyols having more than two aliphatically bound hydroxyl groups, e.g. tris(hydroxymethyl)methylamine
- the abovementioned compounds VI are condensed with a carboxylic acid or sulfonic acid VII which contains at least one free-radically polymerizable functional group or a derivative thereof or a mixture of two or more thereof, in which reaction at least one, preferably all, of the free groups capable of condensation within the compounds VI are condensed with the compound VII.
- Carboxylic acids or sulfonic acids VII which can be used for the purposes of the present invention are in principle all carboxylic and sulfonic acids which contain at least one free-radically polymerizable functional group, and also their derivatives.
- derivatives used here encompasses both compounds which are derived from a carboxylic or sulfonic acid and in which the acid function is modified, e.g. esters, acid halides or acid anhydrides, and compounds which are derived from a carboxylic or sulfonic acid and in which the carbon skeleton of the carboxylic or sulfonic acid is modified, e.g. halocarboxylic or halosulfonic acids.
- Examples of compound VII are, in particular: ⁇ , ⁇ -unsaturated carboxylic acids or j ⁇ , ⁇ -unsaturated carboxylic acids.
- Particularly suitable a,/3-unsaturated carboxylic acids are those of the formula
- R 1 , R 2 and R 3 are hydrogen or C 1 -C 4 -alkyl radicals; among these, preference is in turn given to acrylic acid and methacrylic acid; other suitable compounds are cinnamic acid, maleic acid, fumaric acid, itaconic acid or p-vinylbenzoic acid, and also derivatives thereof, e.g. anhydrides such as maleic anhydride or itaconic anhydride; halides, in particular chlorides, such as acryloyl or methacryloyl chloride; esters such as (cyclo)alkyl (meth)acrylates having up to 20 carbon atoms in the alkyl radical, e.g.
- glyceryl di(meth)acrylate trimethylolpropane di(meth)acrylate, pentaerythrityl di- or tri(meth)acrylate, diethylene glycol bis(mono(2-acryloxy- ethyl)carbonate), poly(meth)acrylates of alcohols which themselves in turn contain a free-radically polymerizable group, e.g. esters of (meth)acrylic acid and vinyl and/or allyl alcohol; vinyl esters of other aliphatic or aromatic carboxylic acids, e.g.
- vinylacetic acid 2-methylvinylacetic acid, isobutyl 3-butenoate, allyl 3-butenoate, allyl 2-hydroxy-3-butenoate, diketene; sulfonic acids such as vinylsulfonic acid, allylsulfonic and methylylsulfonic acids, and also their esters and halides, vinyl benzenesulfonate, 4-vinylbenzenesulfonamide.
- compound X which is capable of free-radical polymerization and can be used for preparing the polymer IX are: olefinic hydrocarbons such as ethylene, propylene, butylene, isobutene, hexene or higher homologues and vinylcyclohexane;
- (meth)acrylonitrile halogen-containing olefinic compounds such as vinylidene fluoride, vinylidene chloride, vinyl fluoride, vinyl chloride, hexafluoropropene, trifluoropropene, 1 ,2-dichloroethylene, 1,2-difluoroethylene and tetrafluoroethylene; vinyl alcohol, vinyl acetate, N-vinylpyrrolidone, N-vinylimidazole, vinylformamide; phosphonitrilic chlorides such as hexachloro(triphosphazene), and also derivatives thereof which are partially or completely substituted by alkoxy, phenoxy, amino and fluoroalkoxy groups, i.e.
- halogen-containing olefinic compounds such as vinylidene fluoride, vinylidene chloride, vinyl fluoride, vinyl chloride, hexafluoropropene, trifluoropropene, 1 ,2-dichloroethylene, 1,2-
- Both these compounds X and the condensation products V . are polymerized by conventional methods well known to those skilled in the art, preferably polymerized by a free-radical mechanism; as regards the molecular weights obtained, what is said below for the compound VIII applies.
- Suitable compounds VIII are, first and foremost, compounds having a mean molecular weight (number average) of at least 5000, preferably from 5000 to 20,000,000, in particular from 100,000 to 6,000,000, which are able to solvate lithium cations and function as binders.
- suitable compounds VIII are polyethers and copolymers which comprise at least 30% by weight of the following structural unit, based on the total weight of the compound VIII:
- R 1 , R 2 , R 3 and R 4 are aryl groups, alkyl groups, preferably methyl groups, or hydrogen and can be identical or different and contain heteroatoms such as oxygen, nitrogen, sulfur or silicon.
- the compound VIII can also consist of a mixture of two or more such compounds.
- the above-defined polymeric composition IV or the polymer IX can also be in the form of a foam, in which case the solid III is present as a dispersion therein.
- the mixes Ila should, according to the present invention, consist of from 1 to 95 % by weight, preferably from 25 to 90% by weight and in particular from 30 to 70% by weight, of a solid III and from 5 to 99% by weight, preferably from 10 to 75 % by weight and in particular from 30 to 70% by weight, of a polymeric composition IV, and the compound VIII of the polymeric composition IV should advantageously have a mean molecular weight (number average) of from 5000 to 100,000,000, preferably from 50,000 to 8,000,000.
- the polymeric composition IV can be obtained by reacting from 5 to 100% by weight, preferably from 30 to 70% by weight, based on the polymeric composition IV, of a compound V with from 0 to 95 % by weight, in particular from 30 to 70% by weight, based on the polymeric composition IV, of a compound VIII.
- the mixes lib should, according to the present invention, consist of from 1 to 95 % by weight, preferably from 25 to 90% by weight and in particular from 30 to 70% by weight, of a solid III and from 5 to 99% by weight, preferably from 10 to 75 % by weight and in particular from 30 to 70% by weight, of a polymer IX, and the compound VIII of the polymer
- the polymer IX should advantageously have a mean molecular weight (number average) of from 5000 to 100,000,000, preferably from 50,000 to 8,000,000.
- the polymer IX can be obtained by reacting from 5 to 75 % by weight, preferably from 30 to 70% by weight, based on the polymer IX, of a compound
- mixture used according to the present invention which should comprise a mix used according to the present invention in an amount of from 1 to 100% by weight, preferably from 35 to 100% by weight and in particular form 30 to 70% by weight, based on the mixture used according to the present invention, a mixture of a solid III, a condensation product V and, if desired, a compound VIII or a mixture of a solid III, a compound X, a compound VIII and customary additives such as plasticizers, preferably plasticizers comprising polyethylene oxide or polypropylene oxide, can be prepared.
- plasticizers preferably plasticizers comprising polyethylene oxide or polypropylene oxide
- polymeric binder used within this second layer B particular mention may be made of the following polymers:
- Polycarbonates such as polyethylene carbonate, polypropylene carbonate, polybutadiene carbonate, polyvinylidene carbonate.
- Polyurethanes for example obtainable by reacting a) organic dusocyanates having from 6 to 30 carbon atoms, for example aliphatic acyclic dusocyanates such as hexamethylene 1,5- diisocyanate and hexamethylene 1,6-diisocyanate, aliphatic cyclic dusocyanates such as cyclohexylene 1 ,4-diisocyanate, dicyclohexylmethane diisocyanate and isophorone diisocyanate or aromatic dusocyanates such as tolylene 2,4-diisocyanate, tolylene 2,6-diisocyanate, m-tetramethylxylene diisocyanate, p- tetramethylxylene diisocyanate, tetrahydronaphthylene 1,5- diisocyanate and diphenylmethane 4,4'-diisocyanate or mixtures of such compounds,
- polyhydric alcohols such as polyesterols, polyetherols and diols.
- the polyesterols are advantageously predominantly linear polymers having terminal OH groups, preferably those having two or three, in particular two, OH end groups.
- the acid number of the poly- esterols is less than 10 and preferably less than 3.
- the polyesterols can be prepared in a simple manner by esterification of aliphatic or aromatic dicarboxylic acids having from 4 to 15 carbon atoms, preferably from 4 to 6 carbon atoms, with glycols, preferably glycols having from 2 to 25 carbon atoms, or by polymerization of lactones having from 3 to 20 carbon atoms.
- dicarboxylic acids which can be used are glutaric acid, pimelic acid, suberic acid, sebacic acid, dodecanoic acid and preferably adipic acid and succinic acid.
- Suitable aromatic dicarboxylic acids are terephthalic acid, isophthalic acid, phthalic acid or mixtures of these dicarboxylic acids with other dicarboxylic acids, e.g. diphenic acid, sebacic acid, succinic acid and adipic acid.
- the dicarboxylic acids can be used individually or as mixtures.
- To prepare the polyesterols it may be advantageous to use the corresponding acid derivatives such as carboxylic anhydrides or carboxylic chlorides in place of the dicarboxylic acids.
- Suitable glycols are diethylene glycol, 1,5-pentanediol, 1, 10-decanediol and 2,2,4-trimethylpentane- 1 ,5-diol. Preference is given to using 1 ,2-ethanediol, 1 ,3- propanediol, 2-methylpropane-l ,3-diol, 1 ,4-butanediol, 1 ,6- hexanediol, 2,2-dimethylpropane-l ,3-diol, 1 ,4-dimethylolcyclohexane, 1 ,4-diethanolcyclohexane and ethoxylated or propoxylated products of 2,2-bis(4-hydroxyphenyl)propane (bisphenol A).
- the polyols can be used alone or as a mixture in various mixing ratios.
- Suitable lactones for preparing the polyesterols are, for example, ⁇ , ⁇ - dimethyl- ⁇ -propiolactone, ⁇ -butyrolactone and preferably e-caprolactone.
- the polyetherols are essentially linear substances having terminal hydroxyl groups and containing ether bonds.
- Suitable polyetherols can easily be prepared by polymerization of cyclic ethers such as tetrahydrofuran or by reacting one or more alkylene oxides having from 2 to 4 carbon atoms in the alkylene radical with an initiator molecule containing two active hydrogen atoms in bound form in the alkylene radical.
- suitable alkylene oxides are ethylene oxide, 1,2-propylene oxid, epichlorohydrin, 1 ,2-butylene oxide and 2,3-butylene oxide.
- the alkylene oxides can be used individually, alternately in succession or as a mixture.
- Suitable initiator molecules are, for example, water, glycols such as ethylene glycol, propylene glycol, 1 ,4-butanediol and 1,6- hexanediol, amines such as ethylenediamine, hexamethylenediamine and 4,4'-diaminodiphenylmethane and aminoalcohols such as ethanolamine.
- Suitable polyesterols and polyetherols and their preparation are described, for example, in EP-B 416 386; suitable polycarbonatediols, preferably those based on 1,6-hexanediol, and their preparation are described, for example, in US-A 4 131 731.
- Use can advantageously be made of up to 30% by weight, based on the total mass of the alcohols, of aliphatic diols having from 2 to 20, preferably from 2 to 10, carbon atoms, e.g. 1,2-ethane- diol, 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, 1,5- pentanediol, 1 , 10-decanediol, 2-methylpropane-l,3-diol, 2,2- dimethylpropane-1 ,3-diol, 2-methyl-2-butylpropane-l ,3-diol, 2,2- dimethylbutane-l ,4-diol, 1,4-dimethylolcyclohexane, neopentyl glycol hydroxypivalate, diethylene glycol, triethylene glycol and methyldi- ethanolamine or aromatic-aliphatic or aromatic-cycloaliphatic
- F derivatives and also mixtures of such compounds.
- Use can advantageously be made of up to 5 % by weight, based on the total mass of the alcohols, of aliphatic triols having from 3 to 15, preferably from 3 to 10, carbon atoms, for example trimethylolpropane or glycerol, the reaction product of such compounds with ethylene oxide and/or propylene oxide, and also mixtures of such compounds.
- the polyhydric alcohols may bear functional groups, for example neutral groups such as siloxane groups, basic groups such as, in particular, tertiary amino groups or acid groups or their salts or groups which are easily converted into acid groups; these groups are introduced via a polyhydric alcohol.
- functional groups for example neutral groups such as siloxane groups, basic groups such as, in particular, tertiary amino groups or acid groups or their salts or groups which are easily converted into acid groups; these groups are introduced via a polyhydric alcohol.
- diol components which bear such groups, e.g. N-methyldiethanolamine , diethyl N , N-bis(hydroxy- 5 ethyl)aminomethylphosphonate or 3-sulfopropyl N,N- bis(hydroxyethyl)-2-aminoacetate, or dicarboxylic acids which bear such groups and can be used for the preparation of polyesterols, for example 5-sulfoisophthalic acid.
- Acid groups are, in particular, the phosphoric acid, phosphonic acid, sulfur ic acid, sulfonic acid, carboxyl or ammonium group.
- Groups which are easily converted into acid groups are, for example, ester groups or salts, preferably of the alkali metals 5 such as lithium, sodium or potassium.
- polyesterols themselves; care should be taken to ensure that molecular weights in the range from 10,000 to 2,000,000, preferably from 50,000 to 1,000,000 are obtained. 0
- the layer B is a cathode layer, it comprises an electron-conducting, electrochemically active compound customarily used for cathodes (cathode compound) which is able to release lithium ions on charging, preferably a lithium compound.
- cathode compound an electron-conducting, electrochemically active compound customarily used for cathodes (cathode compound) which is able to release lithium ions on charging, preferably a lithium compound.
- cathode compound an electron-conducting, electrochemically active compound customarily used for cathodes (cathode compound) which is able to release lithium ions on charging, preferably a lithium compound.
- cathode compound an electron-conducting, electrochemically active compound customarily used for cathodes (cathode compound) which is able to release lithium ions on charging, preferably a lithium compound.
- LiCoO 2 LiNiO 2 , LiNi x CO y O 2 , LiNi x CO
- the layer B is an anode layer, it comprises a customary electron- conducting electrochemically active compound known from the prior art 5 (anode compound) which is able to take up lithium ions on charging; particular examples which may be mentioned are: lithium, lithium-containing metal alloys, micronized carbon black, natural and synthetic graphite, synthetic graphitized carbon powder and carbon fibers, oxides such as titanium oxide, zinc oxide, tin oxide, molybdenum oxide, o tungsten oxide, carbonates such as titanium carbonate, molybdenum carbonate and zinc carbonate.
- the layer B When the layer B is used as anode layer, it further comprises up to 20% by weight, based on the total weight of materials present in it (polymeric binder plus anode compound), of conductive black and, if desired, the abovementioned customary additives.
- the layer B When the layer B is used as cathode or for producing a cathode, it further comprises, based on the total weight of the materials present in it (polymeric binder plus cathode compound), from 0.1 to 20% by weight of conductive black.
- bonding layer C it is possible in principle to use all materials which are able to join the first layer or layers, as defined above, and the second layer or layers, as defined above, to one another.
- the bonding layer is, in particular if the layers in question are joined to one another by hot lamination, generally a material which has a melting point which is lower, preferably from 20 to 50°C lower, than those of the first layer or layers or the second layer or layers or the first layer or layers and the second layer or layers.
- the melting point of these materials is generally from 25 to 250°C, preferably from 50 to 200 °C and in particular from 70 to 180°C.
- the bonding layer can also comprise a solid III.
- the amounts of the solid correspond essentially to the amounts specified for the layers A and B, in each case based on the material forming the bonding layer.
- the bonding layer As such materials forming the bonding layer, it is possible to use all materials customarily used as adhesives. Of course, it has to be possible to apply these materials to the layers A and/or B by customary methods of layer formation, for example printing on, casting on, spraying on, extruding, doctor blade coating, etc. Preference is given to using polymeric compounds as materials forming the bonding layer.
- melt adhesives such as those based on ethylene-vinyl acetate copolymers which are generally additionally mixed with resins and/or waxes or paraffins so as to vary their melt flow index, those based on low molecular weight (co)polyethylene, atactic (co)polypropylene, ethylene-acrylic ester copolymers and styrene-butadiene and styrene-isoprene block copolymers, polyisobutylene and also poly(meth)acrylates and polyesters such as polyethylene terephthalate which can likewise in each case be mixed with plasticizers, in particular those mentioned herein, in order to vary their melt flow index; adhesive plastisols which are essentially mixed from a dispersion of finely divided polyvinyl chloride in plasticizers and low molecular weight materials which are reactive under the action of heat and act as bonding agents, e.g.
- polyethylene oxide polyethylene oxide
- polyvinyl ethers such as poly(vinyl methyl ether), poly(vinyl ethyl ether), poly(vinyl propyl ether), poly(vinyl butyl ether), poly (vinyl isobutyl ether); (co)polyacrylates and (co)polymethacrylates, with preference being given to those having relatively long alkyl chains, e.g.
- polybutyl (meth)acrylate or polyhexyl (meth)acrylate polyvinylpyrrolidone
- polyurethanes where the abovementioned polyurethanes can likewise be used
- wax-like (co)polyolefins such as polyethylene, polypropylene and polyisoprene waxes
- rubber-like materials such as polyisobutylene; and also mixtures of two or more thereof.
- the layers A and/or B and/or C can further comprise a plasticizer.
- Plasticizers which can be used are aprotic solvents, preferably those which solvate Li ions, for example dimethyl carbonate, diethyl carbonate, dipropyl carbonate, diisopropyl carbonate, dibutyl carbonate, ethylene carbonate, propylene carbonate; oligoalkylene oxides such as dibutyl ether, di-tert-butyl ether, dipentyl ether, dihexyl ether, diheptyl ether, dioctyl ether, dinonyl ether, didecyl ether, didodecyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, l-tert-butoxy-2-methoxyethane, l-tert-butoxy-2- ethoxyethane, 1,2-dimethoxypropane, 2-methoxyethyl ether, 2-ethoxyethyl ether, diethylene glycol dibutyl
- ester of the formulae (El) to (E5) can be used as plasticizer:
- esters of the formulae (El) to (E5) preference is given to using the phosphoric esters of the formula (E3).
- esters of the formulae (El) to (E5) in which R 1 , R 2 and, if present, R 3 and/or R 4 are identical and are -CH 2 - CH 2 O-CH 3 or (-CH 2 -CH 2 -O) 2 -CH 3 , with preference again being given to the corresponding phosphoric esters.
- esters used herein are, in terms of their properties, extraordinarily well suited as plasticizers for the layers in question and generally have a viscosity at room temperature of ⁇ lOmPas, preferably ⁇ 5 mPas and in particular ⁇ 3 mPas. They generally have boiling points of about 200 °C or above, preferably about 250 °C or above and in particular about 300 °C or above, in each case measured at atmospheric pressure, and have a sufficiently low vapour pressure of from about 10 "5 to about 10° mbar at the temperatures occurring during their use, viz. from about -50 °C to about 150° C. As a result of their boiling points, they can be distilled and can thus be produced in high purity.
- esters are liquid over a wide temperature range at atmospheric pressure, and are generally still liquid down to a temperature of about -30° C, preferably down to about -40°C.
- the esters described here can be used as plasticizers and as solvents in electrolyte systems for Li ion accummulators at at least about 80°C, preferably at least about 120°C, more preferably at least about 150°C.
- esters used according to the invention can also be employed as a mixture with the previously mentioned plasticizers.
- esters used according to the present invention are prepared by conventional methods, as are described, for example, in K. Mura Kami in Chem. High Polymers (Japan), 7 (1950), pp. 188-193 and in H. Steinberg Organoboron Chemistry, Chapter 5, J. Wiley & Sons, N.Y. 1964.
- the acids, acid anhydrides or chlorides such as boric acid, C(0)C1 2 , POCl 3 , SO 2 Cl 2 and SiCl 4 are used as starting materials and are reacted in a known manner with the appropriate monohydric or polyhydric alcohols or etherols.
- the plasticizer content of the respective layer is, based on the mix present therein or the material making up the layer (polymeric binder plus cathode or anode material), from 0 to 200% by weight, preferably from 0 to 100% by weight and more preferably from 0 to 70% by weight.
- the starting materials used for the respective layers can be dissolved or dispersed in an inorganic or preferably organic liquid diluent, where the resulting solution should have a viscosity of preferably from 100 to 50,000 mPas, and subsequently applied in a known manner, for example by spray coating, casting, dipping, spin coating, roller coating or latterpress, gravure, planographic or screen printing or by extrusion, if desired to a support material, i.e. shaped to form a film-like structure. Further processing can be carried out in a customary way, e.g. by removing the diluent and curing the materials.
- Suitable organic diluents are aliphatic ethers, in particular tetrahydrofuran and dioxane, hydrocarbons, in particular hydrocarbon mixtures such as petroleum spirit, toluene and xylene, aliphatic esters, in particular ethyl acetate and butyl acetate, and ketones, in particular acetone, ethyl methyl ketone and cyclohexanone. It is also possible to use combinations of such diluents.
- Suitable support materials are the materials customarily used for electrodes, preferably metals such as aluminum and copper. It is also possible to use coated glass substrates, in particular ITO-coated glass substrates or temporary intermediate supports such as films, in particular polyester films such as polyethylene terephthalate films. Such films can advantageously be provided with a release layer, preferably of polysiloxanes.
- the production of the individual films which then form the layers within the composite of the present invention can be carried out thermoplastically, for example by injection molding, melt casting, pressing, kneading or extrusion, if desired with a subsequent calendering step.
- volatile components such as solvents or plasticizers can be removed.
- crosslinking of the layers can be carried out in a manner known per se, for example by irradiation with ionic or ionizing radiation, an electron beam, preferably at an acceleration voltage of from 20 to 2000 kV and a radiation dose of from 5 to 50 Mrad, UV or visible light, where, in a customary manner, an initiator such as benzil dimethyl ketal or 1,3,5-trimethylbenzoyl-triphenylphosphine oxide can be advantageously added in amounts of, in particular, at most 1 % by weight based on the constituents to be crosslinked in the starting materials and the crosslinking can advantageously be carried out over a period of, in general, from 0.5 to 15 minutes, advantageously under inert gas such as nitrogen or argon; by thermal free-radical polymerization, preferably at above 60°C, where an initiator such as azobisisobutyronitrile can advantageously be added in amounts of, in general, at most 5 % by weight, preferably from 0.05
- the layers described herein can also comprise a dissociable compound containing lithium cations, viz. a conducting salt, and, if desired, further additives such as, in particular, organic solvents, viz. an electrolyte.
- a dissociable compound containing lithium cations viz. a conducting salt
- further additives such as, in particular, organic solvents, viz. an electrolyte.
- Some or all of these materials can be added to the mixture during the production of the layer or can be introduced into the layer after production of the latter.
- Conducting salts which can be used are the generally known conducting salts which are described, for example, in EP-A 0 096 629.
- the conducting salt used is preferably LiPF 6 , LiBF 4 , LiClO 4 , LiAsF 6 , LiCF 3 S0 3 , LiC(CF 3 S0 2 ) 3 , LiN(CF 3 SO 2 ) 2 , LiN(S0 2 C n F 2n+ 1 ) 2 , LiC[(C n F 2n+ 1 )S0 2 ] 3 , Li(C n F 2n+ 1 )S0 3 , where n is in each case from 2 to 20, LiN(S0 2 F) 2 , LiAlCl 4 , LiSiF 6 , LiSbF 6 or a mixture of two or more thereof, with particular preference being given to using LiBF 4 or LiPF 6 as conducting salt.
- These conducting salts are used in amounts of from 0.1 to 50% by weight, preferably from 0.1 to 20% by weight, in particular from 1 to 10% by weight, in each case based on the material forming the respective layer.
- the films/layers forming the composite of the present invention generally have a thickness of from 5 to 500 ⁇ m, preferably from 10 to 500 ⁇ m, more preferably from 10 to 200 ⁇ m.
- the composite preferably in the form of a film, generally has a total thickness of from 15 to 1500 ⁇ m, in particular a total thickness of from 50 to 500 ⁇ m.
- the present invention also provides a process for producing a composite, which comprises joining the first layer or layers A and the second layer or layers B and, if present, the bonding layer or layers to one another by lamination under the action of heat or pressure or heat and pressure, preferably by hot lamination. It should be ensured that, depending on the material used for the bonding layer, joining can always be carried out at room temperature or at temperatures up to 50 °C or by hot lamination. In the hot or cold lamination, all customary techniques such as roller melt methods, simple pressing and extrusion lamination can be employed.
- the temperatures used are generally from about 50°C to about 250°C, preferably from about 70°C to about 200°C and more preferably from about 100°C to about 180°C.
- a process is also provided for producing a composite, which comprises subjecting the first layer or layers or the second layer or layers or the first layer or layers and the second layer or layers to a corona treatment and subsequently joining the first corona-treated layer or layers to the second corona-treated or untreated layer or layers, preferably by hot lamination.
- Corona treatment is a method widely used in surface treatment for roughening/functionalizing surfaces.
- the roughening/functionalization is achieved by electrical charging of the surfaces.
- a generator produces an AC voltage of from about 10 to about 20 KV at a frequency of from about 20 to about 40 KHz and the generator energy is discharged via an electrode system onto the surface of the substrate to be treated, here the layer or layers as defined above, resulting in functionalization/roughening of the treated surface of the layer.
- the present invention further provides a process for producing a composite, which comprises applying at least one bonding layer to the first layer or layers, the second layer or layers or the first layer or layers and the second layer or layers and subsequently joining the first layer or layers to the second layer or layers via the bonding layer or layers, preferably by hot lamination.
- the present invention provides for the use of a composite, as defined above, for producing an electrochemical cell, in a sensor, an electrochromic window, a display, a capacitor or an ion-conducting film.
- Suitable organic electrolytes for this purpose are the compounds discussed above under “plasticizers”, with preference being given to using the customary organic electrolytes, preferably esters such as ethylene carbonate, propylene carbonate, dimethyl carbonate and diethyl carbonate or mixtures of such compounds.
- first electrode layer e.g. cathode
- bonding layer/separator layer/second electrode layer e.g. anode
- the bonding layer can here also assume the function of a separator, so that the latter can be omitted.
- the procedure is, for example, as follows:
- An anode material e.g. graphite, conductive black and PVDF copolymer are first mixed with one another and the resulting mixture is cast onto a
- a cathode material e.g. LiMn 2 O 4 or LiCoO 2 , conductive black and PVDF copolymer are mixed with one another and cast onto an aluminum foil and dried (layer 2).
- a separator layer plus, if desired, at least one bonding layer by hot lamination gives a composite which can be used, in combination with any solid and/or liquid electrolyte, as an electrochemical cell.
- the filling of such composites with an electrolyte and conducting salt can be carried out either before or preferably after bringing together the layers, if desired after provision of suitable collector electrodes, e.g. a metal foil, and even after introduction of the composite into a battery housing.
- suitable collector electrodes e.g. a metal foil
- the particular microporous structure of the layers when using the mixture of the present invention in particular as a result of the presence of the above- defined solid in the respective layers, makes it possible for the electrolyte and the conducting salt to be taken up and the air in the pores to be displaced. Filling can be carried out at from 0°C to about 100°C, depending on the electrolyte used.
- the electrochemical cells of the present invention can be used, in particular, as automobile batteries, instrument batteries, planar batteries or polymer batteries.
- the mixture was then applied at 60°C to a silicone-treated polyethylene terephthalate film by means of a doctor blade having a casting slit of 300 ⁇ m, the toluene was removed over a period of 5 minutes and peeling off the dried coating gave a film having a thickness of about 30 ⁇ m (separator film).
- the anode foil was powdered with Kynar 2811 (copolymer of vinylidene fluoride and hexafluoropropene, from Elf Atochem) and subsequently, at 160°C, intimately joined to the separator film using a model IL12HR laminator from Ibico.
- the separator film was powdered on one side with Kynar 2811. The powdered side was laid on the anode foil. The two sheets were subsequently intimately joined to one another at 160°C using the laminator described in Example 2.
- Example 4
- aqueous polyethylene dispersion (Polygen WI1 , solids content 35% , from BASF) was applied by means of a doctor blade to an untreated polyethylene terephthalate film.
- the polyethylene layer applied in this way had a thickness of 2 ⁇ m.
- the dispersion described in Example 1 was cast onto the PET film which had been pretreated in this way. After drying, the separator film formed was detached from the PET film. The polyethylene-coated side of the separator was laid on the anode foil. The two sheets were subsequently intimately joined to one another at 160°C using the laminator.
- Example 4 The procedure of Example 4 was repeated, but 5 % of Aerosil R812 (Degussa), based on the dispersion, were added to the polyethylene dispersion.
- Example 4 The procedure of Example 4 was repeated, but 5 % of titanium dioxide T805 (Degussa), based on the dispersion, were added to the polyethylene dispersion.
- Example 4 The procedure of Example 4 was repeated, but 5 % of wollastonite Tremin 939 (Quarzwerke), based on the dispersion, were added to the polyethylene dispersion.
- Example 8 A solution of polyethylene oxide in THF was applied by means of a doctor blade to a silicone-treated polyethylene terephthalate film.
- the polyethylene oxide layer applied in this way had a thickness of 2 ⁇ m.
- the dispersion described in Example 1 was cast onto the PET film which had been pretreated in this way.
- the separator film was detached from the PET film.
- the polyethylene oxide-coated side of the separator was laid on the anode foil. The two sheets were subsequently intimately joined to one another at 160°C using the laminator described in Example 2.
- Example 8 The procedure of Example 8 was repeated, but 5 % of Aerosil R812 (Degussa), based on the solution, were added to the polyethylene oxide solution.
- Example 8 The procedure of Example 8 was repeated, but 5 % of titanium dioxide T805 (Degussa), based on the solution, were added to the polyethylene oxide solution.
- Example 8 The procedure of Example 8 was repeated, but 5 % of wollastonite Tremin 939 (Quarzwerke), based on the solution, were added to the polyethylene oxide solution.
- Example 13 The procedure of Example 8 was repeated, but 3% of propylene carbonate, based on the solution, were added to the polyethylene oxide solution.
- Example 13 The procedure of Example 8 was repeated, but 3% of propylene carbonate, based on the solution, were added to the polyethylene oxide solution.
- Example 8 The procedure of Example 8 was repeated, but 3 % of tris(2-ethylhexyl) phosphate, based on the solution, were added to the polyethylene oxide solution.
- Example 8 The procedure of Example 8 was repeated, but 5 % of wollastonite Tremin 939 (Quarzwerke) and 3 % of tris(2-ethylhexyl) phosphate, based on the solution, were added to the polyethylene oxide solution.
- a solution of Acronal 102 (BASF, polybutyl aery late solution in toluene) was applied by means of a doctor blade to a silicone-treated polyethylene terephthalate film.
- the polybutyl acrylate layer applied in this way had a thickness of 2 ⁇ m.
- Example 1 the dispersion described in Example 1 was cast onto the PET film which had been pretreated in this way. After drying, the separator film was detached from the PET film. The polybutyl aery late-coated side of the separator was laid on the anode foil. The two sheets were subsequently intimately joined to one another at 160°C using the laminator.
- Example 14 The procedure of Example 14 was repeated, but 5 % of Aerosil R812 (Degussa), based on the solution, were added to the polybutyl acrylate solution.
- Example 14 The procedure of Example 14 was repeated, but 5 % of titanium dioxide T805 (Degussa), based on the solution, were added to the polybutyl acrylate solution.
- Example 14 The procedure of Example 14 was repeated, but 5 % of wollastonite Tremin 939 (Quarzwerke), based on the solution, were added to the polybutyl acrylate solution.
- a solution of Oppanol B200 (BASF, polyisobutylene dissolved in n-hexane) was applied by means of a doctor blade to a silicone-treated polyethylene terephthalate film.
- the polyisobutylene layer applied in this way had a thickness of 3 ⁇ m.
- the dispersion described in Example 1 was cast onto the PET film which had been pretreated in this way. After drying, the separator film was detached from the PET film.
- the polyisobutylene-coated side of the separator was laid on the anode foil. The two sheets were subsequently intimately joined to one another at 160°C using the laminator.
- Example 21 The procedure of Example 18 was repeated, but 5 % of Aerosil R812 (Degussa), based on the solution, were added to the polyisobutylene solution.
- Example 21 The procedure of Example 18 was repeated, but 5 % of Aerosil R812 (Degussa), based on the solution, were added to the polyisobutylene solution.
- Example 18 The procedure of Example 18 was repeated, but 5 % of titanium dioxide T805 (Degussa), based on the solution, were added to the polyisobutylene solution.
- Example 18 The procedure of Example 18 was repeated, but 5 % of wollastonite Tremin 939 (Quarzwerke), based on the solution, were added to the polyisobutylene solution.
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Abstract
Description
Claims
Priority Applications (5)
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JP2000516380A JP2001520439A (en) | 1997-10-09 | 1998-10-08 | Composite materials suitable for electrochemical cells |
AU12266/99A AU1226699A (en) | 1997-10-09 | 1998-10-08 | Composite suitable for use in electrochemical cells |
EP98955417A EP1029382A1 (en) | 1997-10-09 | 1998-10-08 | Composite suitable for use in electrochemical cells |
CA002305218A CA2305218A1 (en) | 1997-10-09 | 1998-10-08 | Composite suitable for use in electrochemical cells |
KR1020007003825A KR20010031018A (en) | 1997-10-09 | 1998-10-08 | Composite Suitable for Use in Electrochemical Cells |
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DE19744660.4 | 1997-10-09 | ||
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EP (1) | EP1029382A1 (en) |
JP (1) | JP2001520439A (en) |
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Cited By (11)
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EP1058327A2 (en) * | 1999-06-04 | 2000-12-06 | NBT GmbH | Negative electrode for high energy lithium ion cell and method for manufacturing the same |
WO2001071827A2 (en) * | 2000-03-21 | 2001-09-27 | Midwest Research Institute | Method for improving the durability of ion insertion materials |
JP2002083628A (en) * | 2000-09-07 | 2002-03-22 | Bridgestone Corp | Additive for nonaqueous electrolytic solution secondary battery and the nonaqueous electrolytic solution secondary battery |
JP2003513429A (en) * | 1999-10-29 | 2003-04-08 | フラオンホッファー−ゲゼルシャフト ツーァ フェルデルング デーァ アンゲヴァンテン フォルシュング エー.ファオ. | Film for electrochemical structural member and method for producing the film |
EP1302993A2 (en) * | 2001-10-11 | 2003-04-16 | VARTA Microbattery GmbH | Method of manufacturing an electrode-separator unit for galvanic elements |
EP1406339A1 (en) * | 2002-10-04 | 2004-04-07 | Samsung SDI Co. Ltd. | Organic electrolytic solution and lithium battery employing the same |
US6730440B1 (en) | 1999-04-09 | 2004-05-04 | Basf Aktiengesellschaft | Composite body suitable for utilization as a lithium ion battery |
US6991874B1 (en) * | 1998-05-04 | 2006-01-31 | Basf Aktiengesellschaft | Compositions suitable for electrochemical cells |
EP2530768A3 (en) * | 2003-12-18 | 2013-04-03 | Commissariat à l'Énergie Atomique et aux Énergies Alternatives | Lithium secondary battery having both a high electric potential and a high lithium insertion capacity |
JP2013067801A (en) * | 2000-06-15 | 2013-04-18 | Hydro Quebec | Composition, method and device for forming coating on support |
TWI822069B (en) * | 2021-07-15 | 2023-11-11 | 大陸商深圳幀觀德芯科技有限公司 | Battery roll testing method with imaging systems |
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KR100836202B1 (en) * | 2006-12-29 | 2008-06-09 | 김형원 | Nano polymer-clay, battery and method for producing the battery using thereof |
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- 1998-10-08 JP JP2000516380A patent/JP2001520439A/en active Pending
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Cited By (15)
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US6991874B1 (en) * | 1998-05-04 | 2006-01-31 | Basf Aktiengesellschaft | Compositions suitable for electrochemical cells |
US6730440B1 (en) | 1999-04-09 | 2004-05-04 | Basf Aktiengesellschaft | Composite body suitable for utilization as a lithium ion battery |
EP1058327A3 (en) * | 1999-06-04 | 2005-03-09 | VARTA Automotive Systems GmbH | Negative electrode for high energy lithium ion cell and method for manufacturing the same |
EP1058327A2 (en) * | 1999-06-04 | 2000-12-06 | NBT GmbH | Negative electrode for high energy lithium ion cell and method for manufacturing the same |
JP2003513429A (en) * | 1999-10-29 | 2003-04-08 | フラオンホッファー−ゲゼルシャフト ツーァ フェルデルング デーァ アンゲヴァンテン フォルシュング エー.ファオ. | Film for electrochemical structural member and method for producing the film |
WO2001071827A3 (en) * | 2000-03-21 | 2002-08-29 | Midwest Research Inst | Method for improving the durability of ion insertion materials |
WO2001071827A2 (en) * | 2000-03-21 | 2001-09-27 | Midwest Research Institute | Method for improving the durability of ion insertion materials |
JP2013067801A (en) * | 2000-06-15 | 2013-04-18 | Hydro Quebec | Composition, method and device for forming coating on support |
JP2002083628A (en) * | 2000-09-07 | 2002-03-22 | Bridgestone Corp | Additive for nonaqueous electrolytic solution secondary battery and the nonaqueous electrolytic solution secondary battery |
EP1302993A2 (en) * | 2001-10-11 | 2003-04-16 | VARTA Microbattery GmbH | Method of manufacturing an electrode-separator unit for galvanic elements |
EP1302993A3 (en) * | 2001-10-11 | 2005-03-02 | VARTA Microbattery GmbH | Method of manufacturing an electrode-separator unit for galvanic elements |
EP1406339A1 (en) * | 2002-10-04 | 2004-04-07 | Samsung SDI Co. Ltd. | Organic electrolytic solution and lithium battery employing the same |
US7163767B2 (en) | 2002-10-04 | 2007-01-16 | Samsung Sdi Co., Ltd. | Organic electrolytic solution and lithium battery employing the same |
EP2530768A3 (en) * | 2003-12-18 | 2013-04-03 | Commissariat à l'Énergie Atomique et aux Énergies Alternatives | Lithium secondary battery having both a high electric potential and a high lithium insertion capacity |
TWI822069B (en) * | 2021-07-15 | 2023-11-11 | 大陸商深圳幀觀德芯科技有限公司 | Battery roll testing method with imaging systems |
Also Published As
Publication number | Publication date |
---|---|
WO1999019917A3 (en) | 1999-06-24 |
EP1029382A1 (en) | 2000-08-23 |
KR20010031018A (en) | 2001-04-16 |
CA2305218A1 (en) | 1999-04-22 |
JP2001520439A (en) | 2001-10-30 |
AU1226699A (en) | 1999-05-03 |
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