CN108140833A - 含有甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯的电解质组分及含有该电解质组分的电化学电池 - Google Patents
含有甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯的电解质组分及含有该电解质组分的电化学电池 Download PDFInfo
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- CN108140833A CN108140833A CN201680057784.9A CN201680057784A CN108140833A CN 108140833 A CN108140833 A CN 108140833A CN 201680057784 A CN201680057784 A CN 201680057784A CN 108140833 A CN108140833 A CN 108140833A
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- ring
- carbonate
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 106
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 title claims abstract description 33
- 208000032825 Ring chromosome 2 syndrome Diseases 0.000 title claims description 24
- -1 carboxylate methyl ester Chemical class 0.000 claims abstract description 49
- 239000000654 additive Substances 0.000 claims abstract description 42
- 150000003839 salts Chemical class 0.000 claims abstract description 28
- 239000000010 aprotic solvent Substances 0.000 claims abstract description 8
- 229910052744 lithium Inorganic materials 0.000 claims description 40
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 36
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 35
- 230000000996 additive effect Effects 0.000 claims description 31
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 claims description 26
- 239000003960 organic solvent Substances 0.000 claims description 20
- 239000003575 carbonaceous material Substances 0.000 claims description 19
- 150000005677 organic carbonates Chemical class 0.000 claims description 13
- 125000004122 cyclic group Chemical group 0.000 claims description 12
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 claims description 9
- 239000003063 flame retardant Substances 0.000 claims description 9
- 229910001290 LiPF6 Inorganic materials 0.000 claims description 8
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 5
- 239000006183 anode active material Substances 0.000 claims description 5
- 150000001241 acetals Chemical class 0.000 claims description 4
- 238000005868 electrolysis reaction Methods 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 150000003457 sulfones Chemical class 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 150000004292 cyclic ethers Chemical class 0.000 claims description 3
- 239000003349 gelling agent Substances 0.000 claims description 3
- 239000012744 reinforcing agent Substances 0.000 claims description 3
- 239000003381 stabilizer Substances 0.000 claims description 3
- 239000000080 wetting agent Substances 0.000 claims description 3
- 229910003002 lithium salt Inorganic materials 0.000 claims description 2
- 159000000002 lithium salts Chemical class 0.000 claims description 2
- 125000006091 1,3-dioxolane group Chemical class 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 30
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 30
- 229910001416 lithium ion Inorganic materials 0.000 description 30
- 239000011149 active material Substances 0.000 description 24
- 150000002148 esters Chemical class 0.000 description 20
- 229910002804 graphite Inorganic materials 0.000 description 17
- 239000010439 graphite Substances 0.000 description 17
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- 239000002184 metal Substances 0.000 description 16
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- 239000010703 silicon Substances 0.000 description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 15
- 229910052799 carbon Inorganic materials 0.000 description 15
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- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 10
- 125000000217 alkyl group Chemical group 0.000 description 10
- 229910045601 alloy Inorganic materials 0.000 description 10
- 239000000956 alloy Substances 0.000 description 10
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 10
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- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical group O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 9
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- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 9
- 125000003118 aryl group Chemical group 0.000 description 8
- ZSTLPJLUQNQBDQ-UHFFFAOYSA-N azanylidyne(dihydroxy)-$l^{5}-phosphane Chemical compound OP(O)#N ZSTLPJLUQNQBDQ-UHFFFAOYSA-N 0.000 description 8
- 230000006866 deterioration Effects 0.000 description 8
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- 229910052794 bromium Inorganic materials 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
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- 230000002441 reversible effect Effects 0.000 description 6
- 239000011135 tin Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 5
- 229910020002 S(O)2F Inorganic materials 0.000 description 5
- 229910020005 S(O)2—CmF2m+1 Inorganic materials 0.000 description 5
- 125000003710 aryl alkyl group Chemical group 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 239000011888 foil Substances 0.000 description 5
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- 229910052740 iodine Inorganic materials 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 5
- 229920001515 polyalkylene glycol Polymers 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910052718 tin Inorganic materials 0.000 description 5
- 125000004206 2,2,2-trifluoroethyl group Chemical group [H]C([H])(*)C(F)(F)F 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 125000003342 alkenyl group Chemical group 0.000 description 4
- 125000005599 alkyl carboxylate group Chemical group 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- WVQUCYVTZWVNLV-UHFFFAOYSA-N boric acid;oxalic acid Chemical class OB(O)O.OC(=O)C(O)=O WVQUCYVTZWVNLV-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 4
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 4
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- 125000006656 (C2-C4) alkenyl group Chemical group 0.000 description 3
- 125000006650 (C2-C4) alkynyl group Chemical group 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 125000000882 C2-C6 alkenyl group Chemical group 0.000 description 3
- 125000003601 C2-C6 alkynyl group Chemical group 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 3
- IYDWBHJEYMDOBU-UHFFFAOYSA-N [Li+].[Li+].[Li+].[O-]B([O-])[O-].OC(=O)C(O)=O.OC(=O)C(O)=O Chemical class [Li+].[Li+].[Li+].[O-]B([O-])[O-].OC(=O)C(O)=O.OC(=O)C(O)=O IYDWBHJEYMDOBU-UHFFFAOYSA-N 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 125000000304 alkynyl group Chemical group 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- KWWDVIIKMNQADG-UHFFFAOYSA-N boric acid;difluoro oxalate Chemical compound OB(O)O.FOC(=O)C(=O)OF KWWDVIIKMNQADG-UHFFFAOYSA-N 0.000 description 3
- 125000000480 butynyl group Chemical group [*]C#CC([H])([H])C([H])([H])[H] 0.000 description 3
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 2
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Abstract
一种电解质组分,包括:(i)至少一种有机非质子溶剂;(ii)至少一种导电盐;(iii)甲基‑2‑甲基‑1,3‑二氧戊环‑2‑羧酸甲酯;和(iv)可选地一种或多种添加剂。
Description
技术领域
本发明涉及一种含有甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯的电解质组分,其在电化学电池的电解质组分中的应用及含有该电解质组分的电化学电池。
背景技术
电能储存依然是一项关注度越来越高的主题。电能的有效储存能够使得在其有利时可以发电,当需要时可以使用。二次电化学电池由于具备化学能和电能可逆转换(可充性(rechargeability))的能力,其非常符合这个目的。二次锂电池由于锂离子的原子量小和锂离子的电离能大,能提供高能量密度,因此,二次锂电池在电能储存上获得了特别的关注。并作为电源广泛地用于许多诸如手机、笔记本电脑、迷你照相机等便携式电子设备中。
在二次锂电池中,诸如锂离子电池有机碳酸酯、醚、酯和离子液体被充分用作极性溶剂。本领域中大部分锂离子电池通常含有不止一种溶剂,而是不同有机非质子溶剂的溶剂混合物。常见的溶剂组合物为环状有机碳酸酯和脂肪有机碳酸酯的混合物。环状碳酸酯具有高介电常数,能为用于电解质组分中的导电盐提供高溶解度。脂肪碳酸酯粘度相对较低,加入电解质组分中用于降低粘度及根据其他成分降低电解质组分的熔点。最常用的环状碳酸酯为碳酸亚乙酯和碳酸丙烯酯。碳酸亚乙酯的熔点约为+36℃,因此它在低温下的应用被限制了。碳酸亚乙酯仅能用于含有相对大量如脂肪碳酸酯的低分子有机溶剂的组分中。因为脂肪碳酸酯易燃性相对较高,因此大量脂肪碳酸酯不太好。碳酸丙烯酯的熔点约为-45℃,其在低温下应用非常理想,但其难以与在二次锂离子电池中常用的阳极活性材料石墨合用。碳酸丙烯酯会嵌入用作阳极活性材料的石墨中,从而通过剥落损坏石墨。
在锂离子电池充放电过程中,在不同的电池电位发生各种反应。众所周知,在锂离子电池第一次充电过程中,通常在阳极会生成膜。这种膜通常被称为固体电解质界面膜(SEI)。SEI能渗透锂离子,能保护电解质组分不与阳极直接接触,反之亦然。其由诸如溶剂(如碳酸酯、醚和酯)和阳极表面导电盐(尤其是当阳极活性材料是一种如石墨碳质材料时)的电解质组分的成分还原分解形成的。为了形成SEI,阴极一定量的锂被不可逆的消耗了,且不能被替换。通过加入合适的化合物可能会对SEI的结构和性能产生重大影响,其通过还原很容易在阳极分解,从而在阳极表面形成膜。这也有可能减少不可逆消耗的锂的量。SEI对电化学或光电器件的循环稳定性、储存寿命(calendar ageing)和耐用性(耐高电流)的影响很大。众所周知的一个SEI形成添加剂的例子是碳酸亚乙烯酯。然而,还需要更多的SEI形成添加剂以扩大其应用范围。例如,尽管事实上到现在已知了大量的SEI添加剂,由于碳酸丙烯酯会嵌入石墨结构中,通过这种嵌入会破坏石墨结构,因此碳酸丙烯酯在含有石墨作为阳极活性物质的电化学电池中的应用依然很困难。
US 2014/0220429 A1公开了一种含有碳酸亚乙烯酯和环状1,3-二氧醚的电解质组分,其被氟化烷基和羧酸酯基团取代。碳酸亚乙烯酯和环状1,3-二氧醚是为了抑制非水电解质二次电池的溶胀而添加的。
发明内容
本发明的目的是提供具有如长循环寿命时间(long cycle life time)、储存稳定性(cycle stability)和良好倍率容量(rate capability)等良好电化学性能的电解质组分。本发明的另一个目的是提供可以在宽温度范围内使用的电解质组分,特别是可在低温下使用的电解质组分。本发明的另一个目的是提供可以在低温下使用并具有低可燃性的电解质组分。本发明的另一个目的是提供含有碳酸丙烯酯的电解质组分,其适用于具有长循环寿命时间、储存稳定性和良好倍率容量的二次锂电池中,及提供二次锂电池,其含有易受到作为阳极活性材料的碳酸丙烯酯劣化的碳质材料和含有碳酸丙烯酯的电解质组分。
该目的通过一种电解质组分实现,其包括:
(i)至少一种有机非质子溶剂;
(ii)至少一种导电盐;
(iii)甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯;和
(vi)可选地一种或多种添加剂。
该问题可进一步通过在电解质组分使用甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯,及含有该电解质组分的电化学电池来解决。
含有含甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯的电解质组分的电化学电池表现出良好的循环性能,特别是良好的倍率容量。甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯如此有效以至于即使含有大量碳酸丙烯酯的电解质组分也可用于包含石墨阳极的二次锂电池。甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯作为添加剂的使用使得能提供包含碳酸丙烯酯的电解质组分。这种电解质组分熔点低,能在低温下使用。
具体实施方式
下面对本发明进行详细描述。
根据本发明的电解质组分包括:
(i)至少一种有机非质子溶剂;
(ii)至少一种导电盐;
(iii)甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯;和
(iv)可选地一种或多种添加剂。
该电解质组分优选包括至少一种作为成分(i)的非质子有机溶剂,更优选地至少两种非质子有机溶剂(i)。根据一个实施例,该电解质组分可以含有多达十种非质子有机溶剂。
至少一种非质子有机溶剂(i)优选自环状和脂肪有机碳酸酯、双-C1-C10-烷基醚、双-C1-C4-烷基-C2-C6-亚烷基醚和聚醚、环醚、环状和脂肪缩醛和缩酮、原甲酸酯(orthocarboxylic acids esters)、环状和脂肪羧酸酯、环状和脂肪砜类、环状和脂肪腈和二腈。
更优选地至少一种非质子有机溶剂(i)选自环状和脂肪有机碳酸酯、双-C1-C10-烷基醚、双-C1-C4-烷基-C2-C6-亚烷基醚和聚醚、环状和脂肪缩醛和缩酮、环状和脂肪羧酸酯,再优选地至少一种非质子有机溶剂(i)选自环状和脂肪有机碳酸酯和环状和脂肪羧酸酯,最优选地至少一种非质子有机溶剂(i)选自环状和脂肪有机碳酸酯。特别优选地,电解质组分包括含有至少一种环状有机碳酸酯的至少一种非质子有机溶剂(i),尤其优选地,含有碳酸丙烯酯的至少一种非质子有机溶剂(i)。
根据一个实施例,至少一种非质子有机溶剂(i)包括至少一种脂肪有机碳酸酯和至少一种环状有机碳酸酯,优选地至少一种脂肪有机碳酸酯和碳酸丙烯酯。如果至少一种非质子有机溶剂(i)包括至少一种脂肪有机碳酸酯和至少一种环状有机碳酸酯,脂肪有机碳酸酯与环状有机碳酸酯的质量比优选在1:10至10:1的范围,更优选在4:1至1:4的范围。
根据另一实施例,至少一种非质子有机溶剂(i)包括一种环状有机碳酸酯和至少一种脂肪羧酸酯,优选至少一种羧酸烷基酯和碳酸丙烯酯。如果至少一种非质子有机溶剂(i)包括至少一种羧酸烷基酯和至少一种环状有机碳酸酯,羧酸烷基酯与环状有机碳酸酯的重量比优选在1:10至10:1的范围,更优选在4:1至1:4的范围。羧酸烷基酯优选自C1-C4醇与C1-C4羧酸的酯,例如甲醇、乙醇、异丙醇或正丙醇与甲酸、乙酸或丙酸的酯,例如甲酸甲酯、甲酸乙酯、甲酸异丙酯、甲酸正丙酯、乙酸甲酯、乙酸乙酯、乙酸异丙酯、乙酸正丙酯、丙酸甲酯、丙酸乙酯、丙酸异丙酯和丙酸正丙酯。
若至少一种非质子溶剂(i)包括碳酸丙烯酯,如果碳酸丙烯酯的浓度基于电解质组分的总重至少为10wt.-%(质量百分含量)则是优选地,更优选地至少20wt.-%,再优选地至少30wt.-%。
非质子有机溶剂可以是部分卤代的,例如部分被氟化、氯化或溴化,优选部分被氟化。“部分卤代”指各自分子的一个或多个H被卤原子取代,如F、Cl或Br。优选被F取代。至少一种溶液可选自部分卤代和非卤代非质子有机溶剂,如电解质组分可含有部分卤代和非卤代非质子有机溶剂的混合物。
环状有机碳酸酯的例子为碳酸亚乙酯(EC)、碳酸丙烯酯(PC)和丁烯碳酸酯(BC),其中亚烷基链的一个或多个H可被F和/或C1-C4烷基取代,如4-甲基碳酸亚乙酯、乙烯基氟碳酸酯(FEC)和顺式及反式二氟乙烯碳酸酯。优选环状有机碳酸酯为碳酸亚乙酯、单氟碳酸亚乙酯和碳酸丙烯酯,特别地为碳酸亚乙酯和碳酸丙烯酯。
脂肪有机碳酸酯的例子为双-C1-C10-碳酸烷基酯,其中每个烷基相互独立地优选自双-C1-C4-碳酸烷基酯。例子有如碳酸二乙酯(DEC)、碳酸甲乙酯(EMC)、碳酸二甲酯(DMC)和甲基丙基碳酸酯。优选脂肪有机碳酸酯为碳酸二乙酯(DEC)、碳酸甲乙酯(EMC)和碳酸二甲酯(DMC)。
根据本发明,双-C1-C10-碳酸烷基醚的每个烷基都相互独立地进行选择。双-C1-C10-碳酸烷基醚的例子为二甲基乙醚、乙基甲基醚、二乙醚、甲丙醚、二异丙基醚、二正丁基醚。
双-C1-C4-烷基-C2-C6-亚烷基醚的例子为1,2-二甲氧基乙烷、1,2-二乙氧基乙烷、二甘醇二甲醚(二乙二醇二甲醚)、三甘醇二甲醚(三乙二醇二甲醚)、四甘醇二甲醚(四乙二醇二甲醚)和二乙基乙二醇二乙醚。
合适的聚醚的例子为聚亚烷基二醇,优选聚-C1-C4-亚烷基二醇,尤其聚乙二醇。聚乙二醇可包括摩尔百分量(mol%)高达20mol%的一个或多个共聚形式的C1-C4-亚烷基二醇。聚亚烷基二醇优选为二甲基的或二乙基的封端聚亚烷基二醇。合适的聚亚烷基二醇和更合适的聚乙二醇的摩尔质量Mw可至少为400g/mol。合适的聚亚烷基二醇和更合适的聚乙二醇的摩尔质量Mw可高达5000000g/mol,优选高达2000000g/mol。
环醚的例子为1,4-二氧六环、四氢呋喃及其衍生物,如2-甲基四氢呋喃。
脂肪缩醛的例子为1,1-二甲氧甲烷和1,1-二乙氧基甲烷。环状缩醛的例子为1,3-二氧六环、1,3-二氧戊环及其衍生物,如甲基二氧戊环。
脂肪原甲酸酯的例子为三-C1-C4-烷氧基甲烷,尤其是三甲氧基甲烷和三乙氧基甲烷。合适的环状原甲酸酯的例子为1,4-二甲基-3,5,8-三氧杂双环[2.2.2]辛烷和4-乙基1-甲基-3,5,8-三氧杂双环[2.2.2]辛烷。
脂肪羧酸酯的例子为甲酸乙酯、甲酸甲酯、乙酸乙酯、乙酸甲酯、丙酸乙酯、丙酸甲酯、丁酸乙酯、丁酸甲酯和如1,3-丙二酸二甲酯的二元羧酸酯。环状羧酸酯(内酯)的例子为γ-丁内酯。
环状和脂肪砜类的例子为乙基甲基砜、二甲基砜和四氢噻吩-S-S-二氧化物(环丁砜)。
环状和脂肪的腈和二腈的例子为己二腈、乙腈、丙腈和丁腈。
本发明电解质组分包括至少一种导电盐(ii)。电解质组分作为一种介质可以转移参与电化学电池中发生的电化学反应的离子。电解质中的导电盐(ii)通常溶于非质子有机溶剂(i)。优选地导电盐为锂盐。
导电盐优选自如下组,含有:
Li[F6-xP(CyF2y+1)x],其中,x是范围从0到6的整数,y是范围从1到20的整数;
Li[B(RI)4]、Li[B(RI)2(ORIIO)]和Li[B(ORIIO)2],其中每个RI相互独立地选自F、Cl、Br、I、C1-C4烷基、C2-C4烯基、C2-C4炔基、OC1-C4烷基、OC2-C4烯基和OC2-C4炔基,其中烷基、烯基和炔基可被一个或多个ORIII取代,其中RIII选自C1-C6烷基、C2-C6烯基和C2-C6炔基;和
(ORIIO)是衍生自1,2-或1,3-二醇、1,2-或1,3-二羧酸或1,2-或1,3-羟基羧酸的二价基团,其中二价基团通过两个氧原子与中心B原子形成5元或6元环;
LiClO4、LiAsF6、LiCF3SO3、Li2SiF6、LiSbF6、LiAlCl4、Li(N(SO2F)2)、四氟(草酸)磷酸锂、草酸锂;和
通式为Li[Z(CnF2n+1SO2)m]的盐,其中m和n定义如下:
当Z选自氧和硫时,m=1,
当Z选自氮和磷时,m=2,
当Z选自碳和硅时,m=3,和
n是范围从1到20的整数。
合适的1,2-或1,3-二醇,其衍生物为二价基团(ORIIO),可以为脂肪族的或芳香族的,可以选自,如1,2-苯二酚、丙烷-1,2-二醇、丁烷-1,2-二醇、丙烷-1,3-二醇、丁烷-1,3-二醇、环己基-反式-1,2-二醇和萘-2,3-二醇,其可有选择地被一个或多个F和/或至少一个直链或支链的非氟化、部分氟化或完全氟化的C1-C4烷基取代。1,2-或1,3-二醇的一个例子为1,1,2,2-四(三氟甲基)-1,2-乙二醇。
“完全氟化的C1-C4烷基”是指烷基所有的H原子都被F取代了。
合适的1,2-或1,3-二羧酸,其衍生物为二价基团(ORIIO),可以为脂肪族的或芳香族的,例如草酸、丙二酸(丙烷-1,3-二羧酸)、邻苯二甲酸或间苯二甲酸,优选草酸。1,2-或1,3-二羧酸可选择地被一个或多个F和/或至少一个直链或支链的非氟化、部分氟化或完全氟化的C1-C4烷基取代。
合适的1,2-或1,3-羟基羧酸,其衍生物为二价基团(ORIIO),可以为脂肪族的或芳香族的,例如水杨酸、四氢化水杨酸、羟基丁二酸和2-羟基乙酸,其可有选择地被一个或多个F和/或至少一个直链或支链的非氟化、部分氟化或完全氟化的C1-C4烷基取代。1,2-或1,3-羟基羧酸的一个例子为2,2-双(三氟甲基)-2-羟基-乙酸。
Li[B(RI)4]、Li[B(RI)2(ORIIO)]和Li[B(ORIIO)2]例子为LiBF4、二氟草酸硼酸锂和二草酸硼酸锂。
优选地,至少一种导电盐选自LiPF6、LiBF4和LiPF3(CF2CF3)3,更优选的导电盐选自LiPF6、LiBF4,最优选的导电盐为LiPF6。
至少一种导电盐以最低浓度至少为0.1mol/l存在,基于总电解质组分,优选地至少一种导电盐的浓度为0.5mol/l-2mol/l。
本发明的电解质组分包括作为成分(iii)的甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯,其化学式(I)为
根据本发明的甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯在电解质组分中基于电解质组分总重的浓度通常至少为0.01wt.-%,优选浓度在0.01至90wt.-%的范围,更优选在0.1至30wt.-%的范围。在某些情况下,甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯的浓度可能在通常用于电解质添加剂的范围内,如在0.01至10wt.-%的范围,优选在0.1至7.5wt.-%的范围,更优选在0.1至5wt.-%的范围。在某些情况下,甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯基于电解质组分总重的浓度可以在大于3wt.-%、高至30wt.-%的范围,优选大于5wt.-%、高至30wt.-%。
本发明的另一个目的是甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯在电解质组分中的应用,如作为添加剂和/或作为溶剂的应用。优选地,甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯作为膜形成添加剂用于电解质组分中。在含有碳酸丙烯酯的电解质组分中使用甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯是非常有利的,特别有利的是在用于锂电池的、含有碳酸丙烯酯的电解质组分中使用甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯,该锂电池含有选自容易被碳酸丙烯酯劣化的含碳材料的阳极活性物质。
甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯通常通过将所需量添加到电解质组分中来使用。甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯通常以上述浓度和如优选描述的浓度用于电解质组分中。
根据本发明的电解质组分可选地包括至少一种其他添加剂(iv)。添加剂(iv)可选自SEI形成添加剂、阻燃剂、过充保护添加剂(overcharge protection additive)、润湿剂、HF和/或H2O清除剂、LiPF6盐稳定剂、离子增强剂(ionic solvation enhancer)、缓蚀剂、胶凝剂等。一种或多种添加剂(iv)不同于甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯。
阻燃剂的例子为有机磷化物,如环磷腈、有机磷酰胺、有机亚磷酸盐、有机磷酸盐、有机膦酸酯、有机膦、有机次膦酸盐及其氟化衍生物。
环磷腈的例子为乙氧基五氟环三磷腈(ethoxypentafluorocyclotriphosphazene)(可购自Nippon Chemical Industrial,商标为PhoslyteTME)、六甲基环三磷腈(hexamethylcyclotriphosphazene)和六甲氧基环三磷腈(hexamethoxycyclotriphosphazene),优选为乙氧基五氟环三磷腈。有机磷酰胺的例子为六甲基磷酰胺。有机亚磷酸盐的例子为三(2,2,2-三氟乙基)亚磷酸酯。有机磷酸盐的例子为磷酸三甲盐、磷酸三甲盐、三(2,2,2-三氟乙基)磷酸盐、双(2,2,2-三氟乙基)磷酸甲盐和磷酸三苯盐。有机膦酸酯的例子为膦酸二甲酯、乙基甲基膦酸酯、甲基正丙基膦酸酯、甲基膦酸正丁酯、膦酸二乙酯、乙基正丙基膦酸酯、正丁基膦酸乙酯、膦酸二正丙酯、正丁基膦酸正丙酯、膦酸二正丁酯和双(2,2,2-三氟乙基)甲基膦酸酯。有机膦的例子为三苯基膦。有机次膦酸盐的例子为膦酸二甲酯、次膦酸二乙酯、二正丙基次膦酸酯、三甲基次膦酸酯、三甲基次膦酸酯和三正丙基次膦酸酯。
HF和/或H2O清除剂的例子为可选择地卤代的环状或脂肪的硅胺。
根据本发明的SEI形成添加剂是一种化合物,其在电极上分解以在电极上形成钝化层,可防止电解质组分和/或电极降解。用这种方式,电池的寿命会极大地被延长。术语“SEI”指的是“固体电解质界面膜”。SEI形成添加剂也被命名为膜形成添加剂,这两个术语在本文可相互替换。优选地,SEI形成添加剂在阳极形成钝化层。本发明文中的阳极被定义为电池的负极。优选地,相对于锂,如嵌锂石墨阳极,阳极的还原电位为1伏特或更低。为了确认一种化合物是否适合作为阳极膜形成添加剂,可准备包括石墨电极和例如钴酸锂的锂离子阴极的电化学电池,及含有少量所述化合物的电解液,化合物的量通常是电解质组分的0.1至10wt.-%,优选电解质组分的0.2至5wt.-%。在阳极和阴极之间施加电压时,相对于锂金属基准,记录的电化学电池的差分容量在0.5V和2V之间。如果在第一循环期间观察到显著的微分容量,例如在1V时为-150mAh/V,但在所述电压范围内的任何后续循环中不存在或基本上不存在,则该化合物可被认为是SEI形成添加剂。SEI形成添加剂本身是本领域技术人员公知的。
SEI形成添加剂的例子为碳酸亚乙烯酯及其衍生物(例如碳酸亚乙烯酯和甲基碳酸亚乙烯酯);氟化碳酸乙烯酯及其衍生物(例如单氟化碳酸乙烯酯、顺式或反式双氟碳酸酯);丙磺酸内酯及其衍生物;亚硫酸乙烯酯及其衍生物;草酸盐,其含有如草酸锂,包括草酸二甲酯、双(草酸)硼酸锂、二氟(草酸)硼酸锂、双(草酸)硼酸铵的草酸硼酸盐,包括四氟(草酸)磷酸锂的草酸磷酸盐;和包括式(II)阳离子的离子化合物,
其中,
X是CH2或NRa,
R1选自C1-C6烷基,
R2选自-(CH2)u-SO3-(CH2)v-Rb,
-SO3-是-O-S(O)2-或-S(O)2-O-,优选-SO3-是-O-S(O)2-,
u是从1至8的整数,优选2、3或4,其中,与N原子和/或SO3基团不直接相连的,一个或多个-(CH2)u-烯烃基链的CH2基团,可以被O取代,其中-(CH2)u-烯烃基链的相邻两个CH2基团可以被C-C双键取代,优选地-(CH2)u-烯烃基链没有被取代和u
u是1至8的整数,优选2、3或4,
v是1至4的整数,优选地v为0,
Ra选自C1-C6烷基,
Rb选自C1-C20烷基、C2-C20烯基、C2-C20炔基、C6-C12芳基和C6-C24芳烷基,其可含有一个或多个F,其中,与SO3基团不直接相连的,烷基、烯基、炔基和芳烷基的一个或多个CH2基团,可被O取代,优选地Rb选自C1-C6烷基、C2-C4烯基、C2-C4炔基,其可含有一个或多个F,其中与SO3基团不直接相连的,烷基、烯基、炔基和芳烷基的一个或多个CH2基团,可被O取代,优选的Rb的例子包括甲基、乙基、三氟甲基、五氟代乙酯、正丙基、正丁基、正己基、乙烯基、乙炔基、烯丙基或丙-1-炔基,
且阴离子选自双草酸硼酸盐、二氟(草酸)硼酸盐、[FzB(CmF2m+1)4-z]-、[FyP(CmF2m+1)6-y]-、(CmF2m+1)2P(O)O]-、[CmF2m+1P(O)O2]2-、[O-C(O)-CmF2m+1]-、[O-S(O)2-CmF2m+1]-、[N(C(O)-CmF2m+1)2]-、[N(S(O)2-CmF2m+1)2]-、[N(C(O)-CmF2m+1)(S(O)2-CmF2m+1)]-、[N(C(O)-CmF2m+1)(C(O)F)]-、[N(S(O)2-CmF2m+1)(S(O)2F)]-、[N(S(O)2F)2]-、[C(C(O)-CmF2m+1)3]-、[C(S(O)2-CmF2m+1)3]-,其中m为1至8的整数,z为1至4的整数,y为1至6的整数。
优选地阴离子为双草酸硼酸盐、二氟(草酸)硼酸盐、[F3B(CF3)]-、[F3B(C2F5)]-、[PF6]-、[F3P(C2F5)3]-、[F3P(C3F7)3]-、[F3P(C4F9)3]-、[F4P(C2F5)2]-、[F4P(C3F7)2]-、[F4P(C4F9)2]-、[F5P(C2F5)]-、[F5P(C3F7)]-或[F5P(C4F9)]-、[(C2F5)2P(O)O]-、[(C3F7)2P(O)O]-或[(C4F9)2P(O)O]-、[C2F5P(O)O2]2-、[C3F7P(O)O2]2-、[C4F9P(O)O2]2-、[O-C(O)CF3]-、[O-C(O)C2F5]-、[O-C(O)C4F9]-、[O-S(O)2CF3]-、[O-S(O)2C2F5]-、[N(C(O)C2F5)2]-、[N(C(O)(CF3)2]-、[N(S(O)2CF3)2]-、[N(S(O)2C2F5)2]-、[N(S(O)2C3F7)2]-、[N(S(O)2CF3)(S(O)2C2F5)]-、[N(S(O)2C4F9)2]-、[N(C(O)CF3)(S(O)2CF3)]-、[N(C(O)C2F5)(S(O)2CF3)]-或[N(C(O)CF3)(S(O)2-C4F9)]-、[N(C(O)CF3)(C(O)F)]-、[N(C(O)C2F5)(C(O)F)]-、[N(C(O)C3F7)(C(O)F)]-、[N(S(O)2CF3)(S(O)2F)]-、[N(S(O)2C2F5)(S(O)2F)]-、[N(S(O)2C4F9)(S(O)2F)]-、[C(C(O)CF3)3]-、[C(C(O)C2F5)3]-或[C(C(O)C3F7)3]-、[C(S(O)2CF3)3]-、[C(S(O)2C2F5)3]-和[C(S(O)2C4F9)3]-。
更优选的阴离子选自双草酸硼酸盐、二氟(草酸)硼酸盐、CF3SO3 -和[PF3(C2F5)3]-。
此处使用的术语“C2-C20烯基”是指有2到20个碳原子、一个自由价的不饱和直链或支链碳氢基团。不饱和是指烯基含有至少一个C-C双键。C2-C6烯基包括例如乙烯基、1-丙烯基、2-丙烯基、1-正丁烯基、2-正丁烯基、异丁烯基、1-戊烯基、1-己烯基、1-庚烯基、1-辛烯基、1-壬烯基、1-正癸烯基等。优选C2-C10烯基,更优选C2-C6烯基,再优选C2-C4烯基,特别地乙烯基和1-丙烯-3-基(烯丙基)。
此处使用的术语“C2-C20炔基”是指有2到20个碳原子、一个自由价的不饱和的直链或支链碳氢基团,其中碳氢基团含有至少一个C-C三键。C2-C6炔基包括例如乙炔基、1-丙炔基、2-丙炔基、1-正丁炔基、2-正丁炔基、异丁炔基、1-戊炔基、1-己炔基、-庚炔基、1-辛炔基、1-壬炔基、1-正癸炔基等。优选C2-C10炔基,更优选C2-C6炔基,再优选C2-C4炔基,特别地优选乙炔基和1-丙炔-3-基(炔丙基)。
此处使用的术语“C6-C12芳基”是指有一个自由价的芳香族6至12元碳氢环或稠环。C6-C12芳基的例子为苯基和萘基。优选苯基。
此处使用的术语“C7-C24芳烷基”是指由一个或多个C1-C6烷基取代的芳香族6-12元芳香族碳氢环或稠芳香环。C7-C24芳烷基总共包括7-24个C原子及一个自由价。自由价可位于芳香环或C1-C6烷基上,如C7-C24芳烷基可通过芳烷基的芳香部分或烷基部分结合。C7-C24芳烷基的例子为甲基苯基、苄、1,2-二甲基苯基、1,3-二甲基苯基、1,4-二甲基苯基、乙基苯基、2-丙基苯基等。
WO 2013/026854 A1详细描述了式(II)化合物及其制备。根据本发明优选的式(II)化合物的实例公开于WO 2013/026854A1的第12页第21行至第15页第13行。
优选的SEI形成添加剂为草酸硼酸盐、氟化碳酸乙烯酯及其衍生物、碳酸亚乙烯酯及其衍生物和式(II)化合物。更优选的为双(草酸)硼酸锂、碳酸亚乙烯酯、单氟碳酸乙烯酯和式(II)化合物,特别地为双(草酸)硼酸锂、单氟碳酸乙烯酯和式(II)化合物。若电解质组分含有SEI形成添加剂(iv),其浓度通常为从电解质组分的0.1至10wt.-%,优选从0.2至5wt.-%。
过充保护添加剂的例子为式(III)化合物:
R3为环己基或C6-C12芳基,其可被一个或多个相互独立地选自F、Cl、Br、I、C6-C12芳基和C1-C6烷基的取代基取代,其中C6-C12芳基和C1-C6烷基可被一个或多个相互独立地选自F、Cl、Br和I的取代基取代;和
R4、R5、R6、R7和R8可相同或不同,相互独立地选自H、F、Cl、Br、I、C6-C12芳基和C1-C6烷基,其中C6-C12芳基和C1-C6烷基可被一个或多个相互独立地选自F、Cl、Br和I的取代基取代。
式(III)化合物的例子为环己基苯、联苯、邻三联苯和对三联苯,优选的式(III)化合物为环己基苯和联苯。胶凝剂的例子为聚合物如聚偏二氟乙烯、聚乙二烯-六氟丙烯共聚物、聚乙二烯-六氟丙烯-三氟氯乙烯共聚物、全氟磺酸、聚氧乙烯、聚甲基丙烯酸甲酯、聚丙烯腈、聚丙烯、聚苯乙烯、聚丁二烯、聚乙二醇、聚乙烯吡咯烷酮、聚苯胺、聚吡咯和/或聚噻吩。这些聚合物加入电解液中是为了将液态电解质转换为准固态或固态电解质,从而提高溶剂滞留性,尤其是老化时。
作为添加剂(iv)加入的化合物在电解质组分和含有电解质组分的设备中有多个作用。如,草酸硼酸锂可作为加强SEI形成的添加剂加入,也可作为导电盐加入。
根据本发明的一个实施例,电解质组分含有至少一种添加剂(iv)。优选地,该电解质组分含有至少一种添加剂(iv),其选自膜形成添加剂、阻燃剂、过充保护添加剂、润湿剂、HF和/或H2O清除剂、LiPF6盐稳定剂、离子增强剂、缓蚀剂、胶凝剂等,更优选地电解质组分含有至少一种阻燃剂,再优选地电解质组分含有至少一种选自环磷腈、有机磷酰胺、有机亚磷酸盐、有机膦酸酯、有机膦、有机次膦酸盐的阻燃剂,特别地,电解质组分含有环磷腈。
在电解质组分含有一种或多种阻燃剂的情况下,电解质组分优选含有基于电解质组分总重总共1至10wt.-%的一种或多种阻燃剂,更优选地2至5wt.-%的一种或多种阻燃剂。
根据另一个实施例,电解质组分基本不含碳酸亚乙烯酯。“基本不含”意味着基于电解质组分总重,优选少于0.1wt.-%,更优选少于0.05wt.-%,最优选少于0.01wt.-%。
优选的电解质组分含有基于电解质组分总重的:
(i)至少9.9wt.-%的至少一种有机非质子溶剂;
(ii)0.1至25wt.-%的至少一种导电盐;
(iii)0.01至90wt.-%的甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯;和
(iv)0至25wt.-%的至少一种添加剂。
本发明电解质组分的水含量,基于电解质组分重量优选低于100ppm,更优选低于50ppm,最优选低于30ppm。水含量可根据卡尔费休法通过滴定测得,如DIN 51777或ISO760:1978所述。
本发明电解质组分的HF含量,基于电解质组分的重量优选低于60ppm,更优选低于40ppm,最优选低于20ppm。HF的含量可根据电势量或电势图滴定法(potentiometric orpotentiographic titration method)通过滴定测得。
本发明的电解质组分在工作状态优选液体,更优选1巴、25℃的液体,再优选电解质组分是1巴、-10℃的液体,特别地电解质组分是1巴、-25℃的液体,再优选电解质组分是1巴、-35℃的液体。
本发明的电解质组分可通过本领域(电解质制备领域)技术人员公知的方法制备,总体来说是通过将导电盐(ii)溶解于相应的溶剂(i)混合物中,并加入甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯(iii),及可选添加剂(iv),如上所述。
该电解质组分可用于电化学电池,优选地用于锂电池、双层电容器或锂离子电容器,更优选地用于锂电池,再优选地用于二次锂电池,最优选地用于二次锂离子电池。
本发明进一步提供含有如上所述或被描述为优选的电解质组分的电化学电池。
该电化学设备的总结构已知或本领域(如电池领域)技术人员熟知,例如记载在电池的林登手册上(Linden's Handbook of Batteries)(ISBN 978-0-07-162421-3)。
该电化学电池可以为锂电池、双层电容器或锂离子电容器。
优选地电化学电池为锂电池。此处所用的术语“锂电池”是指电化学电池,其中阳极包括锂金属或锂离子(有时在充/放电时)。阳极可包括锂金属或锂金属合金、封闭和释放(occluding and releasing)锂离子的材料或其他含有化合物的锂,如该锂电池可以为锂离子电池、锂/硫电池或锂/硒硫电池。
特别地优选的电化学设备为锂离子电池,即:二次锂离子电化学电池,其含有阴极活性材料的阴极和含有阳极活性材料的阳极,该阴极活性材料和该阳极活性材料可可逆的封闭和释放锂离子。术语“二次锂离子电化学电池”和“(二次)锂离子电池”在本发明中可相互替换。
至少一种阴极活性材料优选包括可以封闭和释放锂离子的材料,选自锂化过渡金属磷酸盐和锂离子嵌入金属氧化物(lithium ion intercalating metal oxides)。
锂化过渡金属磷酸盐的例子为LiFePO4和LiCoPO4,锂离子嵌入金属氧化物的例子为LiCoO2、LiNiO2、LiMnO2、通式为Li(1+z)[NiaCobMnc](1-z)O2+e的混合层状过渡金属氧化物(其中z为0至0.3,a、b和c可以相等或不相等,其相互独立地为0至0.8,其中a+b+c=1及-0.1≤e≤0.1)、如LiMnO4的含锰尖晶石和通式为Li1+tM2-tO4-d(其中d为0至0.4,t为0至0.4,M是Mn,至少一个额外金属选自含有Co和Ni的组)和Li(1+g)[NihCoiAlj](1-g)O2+k的尖晶石。g、h、i、j和k的代表值为:g=0、h=0.8-0.85、i=0.15-0.20、j=0.02-0.03、k=0。
阴极可进一步包括导电材料,如导电碳和常用组分如粘结剂。适于作为导电材料和粘结剂的化合物对本领域技术人员来说是公知的。例如阴极可含有导电多晶相的碳,例如选自石墨、炭黑、碳纳米管、石墨烯或至少两种上述物质的混合物。此外,阴极可包括一种或多种粘结剂,例如一种或多种有机聚合物,如聚乙烯、聚丙烯腈、聚丁二烯、聚丙烯、聚苯乙烯、聚丙烯酸酯、聚乙烯醇、聚异戊二烯和至少两种共聚单体的共聚物,共聚单体选自乙烯、丙烯、苯乙烯、(甲基)丙烯腈、1,3-丁二烯,特别地,丁苯聚合物和卤代(共)聚物(如聚氯化乙二烯、聚氯化乙烯、聚氟乙烯、聚偏二氟乙烯(PVdF)、聚四氟乙烯、四氟乙烯和六氟丙烯的共聚物、四氟乙烯和偏二氟乙烯的共聚物、聚丙烯腈)。
本发明锂电池的阳极包括能可逆的封闭和释放锂离子或可以与锂形成合金的阳极活性材料。例如,能可逆的封闭和释放锂离子的碳质材料可用作阳极活性材料。合适的碳质材料为结晶碳(如石墨材料,更特别地,天然石墨、石墨化焦、石墨化中间相碳微球(graphitized MCMB)和石墨化中间相沥青基碳纤维(graphitized MPCF))、无定形碳(如焦炭、在低于1500℃燃烧的中间相碳微球(MCMB)、中间相沥青基碳纤维(MPCF))、硬碳和碳酸阳极活性材料(热分解碳、焦炭、石墨,如碳复合材料、可燃有机聚合物和碳纤维)。如果电解质组分中存在碳酸丙烯酯,那么可用作阳极活性材料的一些碳质材料易于被碳酸丙烯酯劣化。这种劣化通常是由于在电池的电化学循环过程中碳酸丙烯酯分子嵌入碳质材料中引起的。丙烯分子的嵌入导致碳质材料的层剥落。例如由于碳酸丙烯酯的嵌入,石墨材料容易被剥落而损坏。通常包含至少部分石墨层的碳质材料在循环过程中容易发生由电解质组分中存在的碳酸丙烯酯引起的这种劣化。为了确认碳质材料是否容易发生由碳酸丙烯酯引起的劣化,可按照下述过程进行:
为了确定碳质材料是否对由碳酸丙烯酯引起的劣化敏感,可以按照以下在实验部分中描述的过程来制备硬币纽扣电池。用碳质材料基电极取代在过程中描述的石墨电极作为负电极。作为电解质,必须使用PC:DMC(1:1,质量比)的1M LiPF6溶液。对碳酸丙烯酯引起的劣化敏感的碳质材料表现出强烈的容量衰减,并且在20次循环后具有低于基于电池的理论容量的25%的容量保持率。
加入甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯能有效防止碳酸丙烯酯引起的碳质阳极活性材料的劣化。根据本发明的一个实施例,阳极活性材料选自易于被碳酸丙烯酯劣化的碳质材料。优选地,阳极活性材料选自含有至少部分石墨层的碳质材料,更优选地阳极活性材料选自石墨材料。
其他的阳极活性材料为锂金属或含有可与锂形成合金的元素的材料。含有可与锂形成合金的元素的材料的非限制性例子包括金属、半金属或其合金。应该理解的是此处使用的术语“合金”是指含有两种或以上金属的合金及一种或多种金属与一种或多种半金属一起的合金。如果一种合金作为整体具有金属性,该合金可能含有非金属元素。在合金的结构中,固体溶液、共晶(共晶混合物)、金属间化合物或其两种或更多共存。这种金属或半金属元素的例子包括但不限制于,钛(Ti)、锡(Sn)、铅(Pb)、铝、铟(In)、锌(Zn)、锑(Sb)、铋(Bi)、镓(Ga)、锗(Ge)、砷(As)、银(Ag)、铪(Hf)、锆(Zr)、钇(Y)和硅(Si)。在元素的长形元素周期表中第4或14族的金属和半金属元素更优选,特别优选的为钛、硅和锡,特别地为硅。锡合金的例子包括一种含有,作为除了锡的第二种组成元素,一种或多种选自含有硅、镁(Mg)、镍、铜、铁、钴、锰、锌、铟、银、钛(Ti)、锗、铋、锑和铬(Cr)的组的元素。硅合金的例子包括一种含有,作为除了硅的第二种组成元素,一种或多种选自含有锡、镁、镍、铜、铁、钴、锰、锌、铟、银、钛、锗、铋、锑和铬的组的元素。
其他可能的阳极活性材料为能嵌入锂离子的硅。硅可以使用不同的形式,如纳米线、纳米管、纳米粒子、薄膜、纳米多孔硅或硅纳米管形式。硅可以沉积在集电器上。集电器可以是金属丝、金属网格、金属网、金属片、金属箔或金属板。优选的集电器为金属箔,如铜箔。硅薄膜可通过被本领域技术人员所熟知的任何技术沉积在金属箔上,例如通过溅射技术。制备硅薄膜电极的一种可能方法请见R.Elazari et al.;Electrochem.Comm.2012,14,21-24。根据本发明,也可使用硅/碳复合材料作为阳极活性材料。
其他可能的阳极活性材料为Ti的锂离子嵌入氧化物。
优选的阳极活性材料选自可逆的封闭和释放锂离子的碳质材料,特别优选的能可逆的封闭和释放锂离子的碳质材料选自易于被碳酸丙烯酯劣化的碳质材料,特别优选的为石墨。在另一优选实施例中,阳极活性材料选自能可逆的封闭和释放锂离子的硅,优选的阳极包括硅薄膜或硅/碳复合材料。在另一优选实施例中,阳极活性材料选自Ti的锂离子嵌入氧化物。
阳极和阴极可以通过制备电极浆液组分和将该浆液组分涂覆在集电器上制得,其中电极浆液组分通过将电极活性材料、粘结剂、可选择的导电材料和增稠剂(若需要)分散在溶液中制得。集电器可以是金属丝、金属网格、金属网、金属片、金属箔或金属板。优选的集电器为金属箔,如铜箔或铝箔。
本发明的锂电池可包括其他常用配件,如隔膜、外壳、连接线缆等。外壳可以是任何形状的,如立方体或圆柱形,棱柱形或使用的外壳为作为袋状加工的金属塑料复合膜。合适的隔膜为例如玻璃纤维隔膜和如聚烯烃隔膜的聚合物隔膜。
若干个本发明的锂电池可以与另外一个相连,如串联或并联。优选串联。本发明进一步提供了将如上所述的本发明的锂离子电池用于设备中,尤其是用于移动设备中。移动设备的例子为车辆,例如汽车、自行车、飞机或如船或舰的水上交通工具。移动设备的其他例子为那些便携式设备,如电脑,尤其是手提式电脑、电话或电力工具,如来自建筑业,尤其是钻头、电动螺丝起子或电动敲平头钉器。但本发明的锂离子电池也可用于固定的能量储存。
即使不进一步说明,可假定本领域技术人员可以在最大程度上应用上述说明。因此,优选的实施例和例子仅用于描述,不会有任何限制的影响。
本发明由如下例子进行解释,但其不对本发明构成限制。
1.电解质组分
电解质组分由甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯(MMDC)、碳酸亚乙酯(EC)、碳酸丙烯酯(PC)、碳酸二甲酯(DMC)、碳酸甲乙酯(EMC)、六氟磷酸锂(LiPF6)和碳酸亚乙烯酯(VC)制成。具体的成分如表2所示。质量百分含量基于电解质组分总重。
2.电化学测试
循环实验:
使用容量为2mAh/cm2的锂镍钴锰氧化物(NCM 523)电极和容量为2.15mAh/cm2的石墨电极组装钮扣电池。使用玻璃纤维过滤隔膜(Whatmann GF/D)作为隔膜,其用100μl各个电解质组分浸泡。所有的电化学测试均在25℃的气候室中进行。根据表1中列出的过程就循环数量测定电池的放电容量。
表1
电化学循环测试的结果示于表2。
表2
表2的结果表明甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯能有效地防止通过嵌入碳酸丙烯酯分子引起的石墨阳极的剥落。包含作为阳极活性物质的石墨和含有甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯及碳酸丙烯酯的电解质组分的电化学电池表现出与包含碳酸丙烯酯作为SEI形成添加剂的基于碳酸丙烯酯的电解质组分的相同电化学电池在100次循环后大致相同的容量保持率。此外,电解质中含有甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯的电池的4C速率放电容量表现出比含有VC作为添加剂的电解质更高。
Claims (14)
1.一种电解质组分,包括:
(i)至少一种有机非质子溶剂;
(ii)至少一种导电盐;
(iii)甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯;和
(vi)可选地一种或多种添加剂。
2.根据权利要求1所述的电解质组分,其特征在于,所述电解质组分包括基于所述电解质组分总重0.01至90wt.-%的甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯(iii)。
3.根据权利要求1或2所述的电解质组分,其特征在于,所述电解质组分包括基于所述电解质组分总重0.1至30wt.-%的甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯(iii)。
4.根据权利要求1-3中任一所述的电解质组分,其特征在于,所述电解质组分中基本不含碳酸亚乙烯酯。
5.根据权利要求1-4中任一所述的电解质组分,其特征在于,所述至少一种非质子有机溶剂(i)选自环状和脂肪有机碳酸酯、双-C1-C10-烷基醚、双-C1-C4-烷基-C2-C6-亚烷基醚和聚醚、环醚、环状和脂肪缩醛和缩酮、原甲酸酯、环状和脂肪羧酸酯和羧酸二酯、环状和脂肪砜类、环状和脂肪腈和二腈。
6.根据权利要求1-5中任一所述的电解质组分,其特征在于,所述至少一种非质子有机溶剂(i)选自环状和脂肪有机碳酸酯。
7.根据权利要求1-6中任一所述的电解质组分,其特征在于,所述至少一种非质子有机溶剂(i)包括碳酸丙烯酯。
8.根据权利要求1-7中任一所述的电解质组分,其特征在于,所述至少一种导电盐(ii)选自锂盐。
9.根据权利要求1-8中任一所述的电解质组分,其特征在于,所述电解质组分包括至少一种添加剂(iv),所述添加剂(iv)选自膜形成添加剂、阻燃剂、过充保护添加剂、润湿剂、HF和/或H2O清除剂、LiPF6盐稳定剂、离子增强剂、缓蚀剂和胶凝剂。
10.根据权利要求1-9中任一所述的电解质组分,其特征在于,所述电解质组分包括基于所述电解质组分总重的:
(i)至少9.9wt.-%的至少一种有机非质子溶剂;
(ii)0.1至25wt.-%的至少一种导电盐;
(iii)0.01至90wt.-%的甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯;和
(iv)0至25wt.-%的至少一种添加剂。
11.甲基-2-甲基-1,3-二氧戊环-2-羧酸甲酯在用于电化学电池的电解质组分中的应用。
12.含有根据权利要求1-10中任一所述电解质组分的电化学电池。
13.根据权利要求14所述的电化学电池,其特征在于,所述电化学电池为锂电池。
14.根据权利要求12或13所述的电化学电池,其特征在于,所述电化学电池包括含有选自碳质材料的阳极活性物质的阳极。
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