CN112470318A - 电解质组合物、电解质膜及电解质膜的制造方法 - Google Patents
电解质组合物、电解质膜及电解质膜的制造方法 Download PDFInfo
- Publication number
- CN112470318A CN112470318A CN201980049424.8A CN201980049424A CN112470318A CN 112470318 A CN112470318 A CN 112470318A CN 201980049424 A CN201980049424 A CN 201980049424A CN 112470318 A CN112470318 A CN 112470318A
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- Prior art keywords
- monomer
- salt
- alkali metal
- electrolyte
- electrolyte membrane
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Abstract
本发明的目的在于提供一种电解质组合物,由该电解质组合物得到的电解质膜的电池性能优于现有技术中的电解质膜。本发明公开了一种电解质组合物,含有碱金属盐,其特征在于:该组合物还含有光固化单体和/或热固化单体、盐解离剂,碱金属盐的含量比例相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总量100质量%在50质量%以上。
Description
技术领域
本发明涉及一种电解质组合物、电解质膜及电解质膜的制造方法。更详细而言,涉及一种含有下述电解质组合物的电解质膜及电解质膜的制造方法,该电解质组合物非常适合用作锂离子电池等的电池材料。
背景技术
近年来,环境问题越来越受到人们的关注,在此背景下,能量资源从石油和煤炭等化石燃料的转换不断得到推进,与此同时,电池的重要性日益凸显,对电池需求预计将会增加。其中,能够反复充放电的二次电池不仅用于手机、笔记本电脑等电子设备,还广泛用于汽车、飞机等各种领域,对各种二次电池、二次电池所使用的材料的研发不断深入。尤其是容量大且重量轻的锂离子电池,它是预期在将来使用最多的二次电池,也是研发最为活跃的电池。
在上述电池的研发中,人们已开发出一种提高全固体电池所使用的电解质的离子电导率的技术。例如,专利文献1公开了一种固体电解质组合物,其含有具有交联性基团的聚醚聚合物、电解质盐化合物以及作为光聚合引发剂以规定结构表示的化合物。此外,专利文献2公开了一种高分子固体电解质,其含有电解质盐和以规定结构表示、分子量在300以下且含碳酸酯基的(甲基)丙烯酸酯单体的聚合物。专利文献3公开了一种电解质材料,以在侧链上具有醚键的聚合物和电解质盐为必需成分,其特征在于:该聚合物含有由单体成分得到的聚合物,该单体成分含有以规定结构表示的单体,该电解质盐含有离子化合物,该离子化合物由碱金属阳离子和选自下述群组的至少一种阴离子构成,该群组由R3SO2N-SO2R4(R3、R4相同或不同,表示F、CF3、C2F5中之任一者)、PF6-、BF4-、CF3SO3-、四氰基硼酸盐组成。
专利文献1:国际公开第2007/119460号公报
专利文献2:日本公开专利公报特开2008-218237号公报
专利文献3:日本公开专利公报特开2011-142073号公报
发明内容
-发明要解决的技术问题-
如上所述,人们已开发出各种电解质组合物等。然而,由现有的电解质组合物形成的电解质膜在电池性能方面还不完善。
本发明正是为解决上述技术问题而完成的,其目的在于:提供一种电解质组合物,由该电解质组合物得到的电解质膜的电池性能优于现有的电解质膜。本发明的目的还在于:提供一种采用上述电解质组合物的电解质膜及电解质膜的制造方法。
-用于解决技术问题的技术方案-
本申请发明人对电解质组合物进行各种研究后发现:使用含有规定量的碱金属盐、光固化单体和/或热固化单体、盐解离剂的组合物而得到的电解质膜能发挥出优于现有的电解质膜的电池性能。具体而言,本申请发明人发现:用含有上述成分的组合物得到的电解质膜的碱金属离子迁移数优异,且在通电试验中提高施加的电流值来对膜施加负荷时,离子电导性也很优异,这样一来,组装有上述电解质膜的电池的放电电压、放电容量就很优异。本申请发明人还发现:含有上述成分的组合物即使不使用溶剂也能够形成电解质膜。像这样,本申请发明人想到能够完美解决上述问题,从而完成了本发明。
即,本发明是一种含有碱金属盐的电解质组合物,所述组合物还含有光固化单体和/或热固化单体、盐解离剂,碱金属盐的含量比例相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总量100质量%在50质量%以上。
优选地,所述碱金属盐由下式(1)表示,
MN(SO2R1)(SO2R2) (1)
(式中,M表示碱金属离子。R1、R2相同或不同,且表示氟原子或碳原子数1~3的氟烷基)。
优选地,所述碱金属盐是双氟磺酰亚胺的碱金属盐。
优选地,所述光固化单体和/或热固化单体具有杂元素。
所述光固化单体和/或热固化单体可以采用一种或多种,优选地,含有多官能单体。
优选地,所述盐解离剂是磺酰基化合物。
优选地,所述盐解离剂是碳酸酯化合物。
优选地,所述盐解离剂是腈化合物。
优选地,所述电解质组合物含有聚合引发剂。
本发明还是一种电解质膜,通过将所述电解质组合物固化而得到,所述电解质膜也是含有碱金属盐、聚合物以及盐解离剂的电解质膜,该聚合物具有源自于光固化单体和/或热固化单体的结构单元。
所述电解质膜也可以含有沸点低于所述盐解离剂的有机溶剂,优选地,所述有机溶剂的含量相对于碱金属盐、聚合物、盐解离剂的总含量100质量%在20质量%以下,该聚合物具有源自于光固化单体和/或热固化单体的结构单元。
本发明还是一种电解质膜的制造方法,所述制造方法也是下述电解质膜的制造方法,包括将所述电解质组合物固化的工序,在所述固化工序中,沸点低于盐解离剂的有机溶剂的用量相对于所述组合物中的碱金属盐、光固化单体和/或热固化单体、盐解离剂的总含量100质量%在20质量%以下。
-发明的效果-
本发明的电解质组合物由上述构成方式构成,得到的电解质膜的电池性能优于现有的电解质膜,因此非常适合用作锂离子电池等的电池材料等。
附图说明
图1示出对在实施例2-1、2-2和比较例2-1中制造的硬币型锂离子二次电池进行了充放电试验后的结果、得到的放电曲线。
具体实施方式
下面对本发明的优选方式进行具体说明,但本发明并不限于下述记载,在不变更本发明主旨的范围内能够做出适当变更后进行应用。需要说明的是,将以下记载的本发明的各种优选方式中的两个或三个以上进行组合而得到的方式也属于本发明的优选方式。
[电解质组合物]
本发明的电解质组合物含有碱金属盐、光固化单体和/或热固化单体以及盐解离剂,碱金属盐的含量比例相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总量100质量%在50质量%以上。由于所述组合物含有上述成分,所以得到的电解质膜的电池性能优异。而且,通过使用所述组合物,能够在没有溶剂的情况下成膜。此外,通过使所述组合物含有光固化单体和/或热固化单体,在将该组合物固化而得到电解质膜时所述单体会聚合,因此得到的电解质膜的机械强度优异,自支撑膜性也很优异。
碱金属盐在所述组合物中的含量比例没有特别限制,优选相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总量100质量%在50质量%以上。由此得到的电解质膜的离子电导性进一步提高。从制膜性的观点出发,现有的电解质组合物很难提高碱金属盐浓度,但在本发明中,通过使组合物含有碱金属盐、光固化单体和/或热固化单体以及盐解离剂,在含有高浓度碱金属盐的情况下,也能够在充分抑制制膜性下降的同时,使离子电导性进一步提高。此外,一般认为:在碱金属盐浓度较高的情况下,由阴离子形成的电导路径与碱金属离子的电导性有很大关系,因此组合物含有盐解离剂,在组合物中解离出碱金属离子与阴离子,这具有特殊的技术意义。碱金属盐的含量比例优选在52质量%以上,更优选在54质量%以上,进一步优选在56质量%以上,特别优选在58质量%以上。此外,所述碱金属盐的含量比例更优选在98质量%以下,进一步优选在95质量%以下,更进一步优选在90质量%以下,特别优选在88质量%以下。
光固化单体和/或热固化单体在所述电解质组合物中的含量没有特别限制,优选相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总量100质量%为10~45质量%。这样一来,即使碱金属盐浓度较高,聚合反应也会充分进行,能够得到机械强度更优异的电解质膜。光固化单体和/或热固化单体的含量更优选为13~43质量%,特别优选为15~40质量%。根据碱金属盐、盐解离剂、聚合引发剂以及其他成分的含量,光固化单体和/或热固化单体的含量也可以为18~38质量%。需要说明的是,在所述电解质组合物含有两种以上光固化单体和/或热固化单体的情况下,该单体的含量表示两种以上单体的总含量。
盐解离剂在所述电解质组合物中的含量没有特别限制,优选相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总量100质量%为0.5~30质量%。这样一来,即使碱金属盐浓度较高,离子也会更充分地解离,离子电导性会进一步提高。更优选为1~28质量%,进一步优选为2~26质量%,更进一步优选为5~25质量%,再进一步优选为8~20质量%,特别优选为10~20质量%。根据碱金属盐、光固化单体和/或热固化单体、聚合引发剂以及其他成分的含量,盐解离剂的含量可以在15质量%以下,也可以在12质量%以下,还可以在10质量%以下。
优选地,所述电解质组合物含有聚合引发剂。这样一来,使用电解质组合物来得到电解质膜时,能够更充分地使电解质组合物固化。聚合引发剂在所述电解质组合物中的含量没有特别限制,优选相对于光固化单体和/或热固化单体100质量%在0.1质量%以上。更优选在0.2质量%以上,进一步优选在0.5质量%以上。此外,聚合引发剂的含量优选在10质量%以下,更优选在9质量%以下,进一步优选在8质量%以下,特别优选在5质量%以下。如果聚合引发剂的含量为0.1~10质量%,则能够在充分抑制电解质膜的特性丧失的同时,更充分地提高膜的强度。
所述电解质组合物也可以含有碱金属盐、光固化单体和/或热固化单体、盐解离剂、聚合引发剂以外的其他成分。
其他成分的含量优选相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总量100质量%为0~30质量%。更优选为0~25质量%,进一步优选为0~15质量%。
下面进一步对本发明的电解质组合物所含有的必需成分和任意成分进行说明。
<碱金属盐>
所述碱金属盐没有特别限制,构成碱金属盐的碱金属例如有锂、钠、钾、铷、铯、钫。优选为锂、钠、钾,更优选为锂。
所述碱金属盐例如有:LiFSO3等氟磺酸的碱金属盐;LiCF3SO3等三氟甲磺酸的碱金属盐;LiN(FSO2)2等酰亚胺系碱金属盐;LiC(CF3SO2)3等全氟烷基磺酰基甲基化物的碱金属盐;LiPFa(CmF2m+1)6-a(0≤a≤6,1≤m≤2)等氟磷酸盐;LiClO4等高氯酸碱金属盐;LiBFb(CnF2n+1)4-b(0≤b≤4,1≤n≤2)等氟硼酸盐;LiBOB等草酸硼酸的碱金属盐;四氰基硼酸锂等氰基硼酸盐;LiAsF6、LiI、LiSbF6等碱金属盐等。
优选为其中的LiN(FSO2)2等酰亚胺系碱金属盐,更优选为由下式(1)表示的化合物,
MN(SO2R1)(SO2R2)(1)
(式中,M表示碱金属离子。R1、R2相同或不同,且表示氟原子或碳原子数1~3的氟烷基)。
上述M中的碱金属如上所述。
上述R1、R2中的碳原子数1~3的氟烷基只要是碳原子数1~3的烃基所具有的至少一个氢原子被氟原子取代后的氟烷基即可。具体而言,例如有氟甲基、二氟甲基、三氟甲基、氟乙基、二氟乙基、三氟乙基、五氟乙基等。R1、R2优选为氟原子、三氟甲基、五氟乙基,更优选为氟原子、三氟甲基,最优选为氟原子。
优选为,上式(1)所表示的化合物中的双氟磺酰亚胺的碱金属盐、双(三氟甲磺酰基)酰亚胺的碱金属盐,更优选为LiN(FSO2)2(LiFSI)、LiN(CF3SO2)2(LiTFSI),进一步优选为LiN(FSO2)2。
当所述电解质组合物含有LiN(FSO2)2和/或LiN(CF3SO2)2时,优选,LiN(FSO2)2和LiN(CF3SO2)2的合计含量相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总量100质量%为50~98质量%。更优选为52~95质量%,进一步优选为55~90质量%。
<光固化单体和/或热固化单体>
光固化单体和/或热固化单体只要具有可通过光和/或热聚合的官能基,便没有特别限制。所述官能基例如有聚合性不饱和基、环氧基、异氰酸酯基等。
光固化单体和/或热固化单体还优选具有杂元素。
杂元素例如有氮、氧、硫、磷、氯、碘、溴等元素,优选为氧、氮,更优选为氧。
光固化单体和/或热固化单体可以具有一个能聚合的官能基,也可以具有两个以上能聚合的官能基。单官能单体例如有:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸3-氯-2-羟基丙酯,(甲基)丙烯酸2-羟基-3-苯氧基丙酯等可以具有取代基的(甲基)丙烯酸烷基酯类;甲氧基(聚)乙二醇(甲基)丙烯酸酯、甲氧基(聚)丙二醇(甲基)丙烯酸酯、苯氧基乙二醇(甲基)丙烯酸酯等烷氧基(聚)亚烷基二醇(甲基)丙烯酸酯类;2-丙烯酰氧乙基琥珀酸、2-丙烯酰氧基乙基四氢邻苯二甲酸、(甲基)丙烯酸等含羧基的单体;叔丁基缩水甘油醚、叔丁基缩水甘油醚、苄基缩水甘油醚、2-乙基己基缩水甘油醚等单官能环氧化合物;乙二醇单烯丙基醚等单官能烯丙基醚化合物等。
具有两个以上能聚合的官能基的多官能单体例如有:1、3-丁二醇二(甲基)丙烯酸酯、(聚)乙二醇二(甲基)丙烯酸酯、(聚)丙二醇二(甲基)丙烯酸酯、(聚)乙烯(聚)丙二醇二(甲基)丙烯酸酯、二噁烷二醇二(甲基)丙烯酸酯、三环癸烷二甲醇二(甲基)丙烯酸酯、乙氧基化双酚A二(甲基)丙烯酸酯、三羟甲基丙烷三(甲基)丙烯酸酯、乙氧基化三羟甲基丙烷三(甲基)丙烯酸酯、丙氧基化三羟甲基丙烷三(甲基)丙烯酸酯、乙氧基化甘油三(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯等多官能(甲基)丙烯酸酯类;(聚)乙二醇二缩水甘油醚、二乙二醇二缩水甘油醚、(聚)丙二醇二缩水甘油醚、1,6-己二醇二缩水甘油醚、(甲基)丙烯酸缩水甘油酯、(甲基)丙烯酸α-甲基缩水甘油酯、(甲基)丙烯酸3,4-环氧环己基甲酯、环氧丁烯、3,4-环氧-1-戊烯、1,2-环氧-5,9-环十二碳二烯、3,4-环氧-1-乙烯基环己烯、1,2-环氧-5-环辛烯、乙烯基缩水甘油醚、烯丙基缩水甘油醚、4-乙烯基环己基缩水甘油醚、α-萜烯缩水甘油醚、环己烯基甲基缩水甘油醚、4-乙烯基苄基缩水甘油醚、4-烯丙基苄基缩水甘油醚、烯丙基缩水甘油醚、乙二醇烯丙基缩水甘油醚、乙二醇乙烯基缩水甘油醚、二甘醇烯丙基缩水甘油醚、二乙二醇乙烯基缩水甘油醚、三乙二醇烯丙基缩水甘油醚、三乙二醇乙烯基缩水甘油醚、低聚乙二醇烯丙基缩水甘油醚、低聚乙二醇乙烯基缩水甘油醚等多官能环氧化合物;(甲基)丙烯酸乙烯氧基乙酯、(甲基)丙烯酸乙烯氧基乙氧基乙酯、1-(甲基)丙烯酰基-4-氰基-4-(甲基)丙烯酰基氨基-2,2,6,6-四甲基哌啶等多官能乙烯基化合物;2-(甲基)丙烯酰氧基乙基异氰酸酯、(甲基)丙烯酰基异氰酸酯、间异丙烯基-α,α二甲基苄基异氰酸酯等含氰酸酯基的化合物、具有氨基甲酸酯键和丙烯酸酯基的氨基甲酸酯丙烯酸酯等。上述物质可以单独使用,也可以两种以上同时使用。
所述光固化单体和/或热固化单体优选含有多官能单体。
所述光固化单体和/或热固化单体还优选具有醚基。更优选具有源自于环氧烷的结构单元。
具有源自于环氧烷的结构单元的光固化单体和/或热固化单体例如有所述(烷氧基)(聚)亚烷基二醇(甲基)丙烯酸酯类、多官能(甲基)丙烯酸酯类、多官能环氧化合物等。
此外,也优选同时使用具有源自于环氧烷的结构单元的光固化单体和/或热固化单体以及其他多官能单体。同时使用的多官能单体优选为聚氨酯丙烯酸酯。
本发明的优选实施方式之一是同时使用具有源自于环氧烷的结构单元的单官能单体和聚氨酯丙烯酸酯的方式。
具有源自于环氧烷的结构单元的单官能单体优选为由下式(2)表示的化合物,
【化学式1】
(式中,R3相同或不同,且表示氢原子或碳原子数1~30的烃基。R4相同或不同,且表示氢原子或甲基。A1O相同或不同,且表示氧化烯基。n1表示数量1~50)。
此外,具有源自于环氧烷的结构单元的多官能单体优选为由下式(3)表示的化合物,
【化学式2】
(式中,R4相同或不同,且表示氢原子或甲基。A2O相同或不同,且表示氧化烯基。n2表示数量1~50)。
上式(2)中的R3是氢原子或碳原子数1~30的烃基。
碳原子数1~30的烃基例如有碳原子数1~30的脂肪族烷基、碳原子数3~30的脂环族烷基、碳原子数6~30的芳基等。
所述脂肪族或脂环族烷基例如有甲基、乙基、正丙基、正丁基、正戊基(戊基)、正己基、正庚基、正辛基、正壬基、正癸基、正十一烷基、正十二烷基、正十三烷基、正十四烷基、正十五烷基、正十六烷基、正十七烷基、正十八烷基、正十九烷基、正二十烷基、异丙基、仲丁基、异丁基、叔丁基、1-甲基丁基、1-乙基丙基、2-甲基丁基、异戊基、新戊基、1,2-二甲基丙基、1,1-二甲基丙基、叔戊基、1,3-二甲基丁基、3,3-二甲基丁基、2-乙基丁基、2-乙基-2-甲基丙基、1-甲基庚基、2-乙基己基、1,5-二甲基己基、叔辛基、支化的壬基、癸基、十二烷基、硬脂基、二十烷基、环丙基、环丙基甲基、环丁基、环丁基甲基、环戊基、环己基、环己基甲基、环庚基、环辛基、环己基丙基、环十二烷基、降冰片基(C7)、金刚烷基(C10)、环戊基乙基等。
所述碳原子数1~30的烷基的碳原子数优选为1~22,更优选为1~18,进一步优选为1~12,更进一步优选为1~8,特别优选为1~4。
碳原子数6~30的芳基例如有:苯基;萘基;苄基、1-苯乙基、2-苯乙基、3-苯丙基,4-苯丁基、苯乙烯基(Ph-CH=C-基)、肉桂基(Ph-CH=CHCH2-基)、1-苯并环丁烯基、1,2,3,4-四氢萘基等芳烷基等。
所述碳原子数6~30的芳基的碳原子数优选为6~20,更优选为6~10。
上式(2)中的A1O、上式(3)中的A2O“相同或不同”,且表示氧化烯基,这意味着存在于聚亚烷基二醇中的n1或n2个氧化烯基可以全部相同也可以不同。
所述氧化烯基是环氧烷加成物,上述环氧烷例如有环氧乙烷、环氧丙烷、环氧丁烷、异环氧丁烷、1-环氧丁烷、2-环氧丁烷、环氧苯乙烷等碳原子数2~8的环氧烷。更优选为环氧乙烷、环氧丙烷、环氧丁烷等碳原子数2~4的环氧烷,进一步优选为环氧乙烷和环氧丙烷。
此外,当所述聚亚烷基二醇是选自环氧乙烷、环氧丙烷、环氧丁烷,环氧苯乙烷等中任意两种以上的环氧烷加成物时,可以是无规加成、嵌段加成、交替加成中的任一方式。而且,聚亚烷基二醇中的氧化烯基优选具有氧化乙烯基作为必需成分,更优选50摩尔%以上是氧化乙烯基,进一步优选80摩尔%以上是氧化乙烯基。
上式(2)中的n1为1~50,优选为2~45,更优选为5~40。
上式(3)中的n2为1~50,优选为2~45,更优选为5~40。
上式(2)、(3)中的R4优选为氢原子或甲基。
具有源自于环氧烷的结构单元的单官能单体更优选为:乙二醇(甲基)丙烯酸酯、二乙二醇(甲基)丙烯酸酯、丙二醇(甲基)丙烯酸酯、二丙二醇(甲基)丙烯酸酯等(聚)亚烷基二醇(甲基)丙烯酸酯;甲氧基(聚)乙二醇(甲基)丙烯酸酯、甲氧基(聚)乙二醇(甲基)丙烯酸酯等烷氧基(聚)亚烷基二醇(甲基)丙烯酸酯。进一步优选为甲氧基(聚)乙二醇(甲基)丙烯酸酯。
具有源自于环氧烷的结构单元的多官能单体更优选为乙二醇二(甲基)丙烯酸酯、二乙二醇二(甲基)丙烯酸酯、三乙二醇二(甲基)丙烯酸酯、丙二醇二(甲基)丙烯酸酯、二丙二醇二(甲基)丙烯酸酯、三丙二醇二(甲基)丙烯酸酯等(聚)亚烷基二醇二(甲基)丙烯酸酯。进一步优选为聚乙二醇二(甲基)丙烯酸酯。
光固化单体和/或热固化单体优选含有如上所述的多官能单体,其含量优选相对于光固化单体和/或热固化单体的总量100质量%为30~100质量%。更优选为40~100质量%,进一步优选为50~100质量%。
此外,光固化单体和/或热固化单体优选含有如上所述的具有源自于环氧烷的结构单元的单体,其含量优选相对于光固化单体和/或热固化单体的总量100质量%为30~100质量%。更优选为40~100质量%,进一步优选为50~100质量%。
此外,从碱金属盐的溶解性的观点出发,具有源自于环氧烷的结构单元的单体的含量相对于光固化单体和/或热固化单体的总量100质量%可以为60~100质量%,也可以为80~100质量%。
光固化单体和/或热固化单体的分子量没有特别限制,优选在4000以下。更优选在3800以下,进一步优选在3500以下。
<盐解离剂>
所述盐解离剂只要能促进碱金属盐解离为离子便没有特别限制,优选为具有杂元素的化合物。
所述具有杂元素的化合物例如有碳酸酯化合物、磺酰基化合物、腈化合物、羧酸酐、硫酸酯化合物、硫醚化合物、亚硫酸酯化合物、含氮链状化合物、含氮环状化合物等。
优选为其中的碳酸酯化合物、磺酰基化合物和/或腈化合物。通过使所述盐解离剂含有碳酸酯化合物、磺酰基化合物和/或腈化合物,能进一步促进碱金属盐向离子解离,使组合物的离子电导性进一步提高。
碳酸酯化合物例如有:碳酸乙烯酯(EC)、碳酸丙烯酯(PC)、碳酸亚乙烯酯(VC)、碳酸乙烯亚乙酯(VEC)、甲基碳酸亚乙烯酯(MVC)、乙基碳酸亚乙烯酯(EVC)等环状碳酸酯;氟代乙烯碳酸酯、三氟代碳酸亚丙酯等氟化环状碳酸酯。优选为其中的碳酸乙烯酯、氟代乙烯碳酸酯,更优选为碳酸乙烯酯。
磺酰基化合物例如有:二甲基砜、乙基甲基砜、二乙基砜、正丙基甲基砜、异丙基甲基砜、正丁基甲基砜、叔丁基甲基砜等砜类;;环丁砜(四亚甲基砜)、2-甲基环丁砜、3-甲基环丁砜、2,4-二甲基环丁砜等环丁砜类;1,3-丙烷磺酸内酯、1,4-丁烷磺酸内酯等磺酸内酯类;白消安、3-环丁烯砜等。磺酰基化合物优选为二甲基砜、3-环丁烯砜和环丁砜。
腈化合物例如有单腈化合物、二腈化合物。
单腈化合物例如有己腈、庚腈、辛腈、壬腈、癸腈、十一烷腈、十二烷腈、环戊烷腈、环己烷腈、丁烯腈、3-甲基丁烯腈、2-甲基-2-丁烯腈、2-戊烯腈、2-甲基-2-戊烯腈、3-甲基-2-戊烯腈、2-己烯腈等。
二腈化合物例如有:丙二腈、丁二腈(succinonitrile)、戊二腈、己二腈、庚二腈、辛二腈、壬二腈、癸二腈、十一烷二腈、十二烷二腈、甲基丙二腈、乙基丙二腈、异丙基丙二腈、叔丁基丙二腈、甲基丁二腈、2,2-二甲基丁二腈、2,3-二甲基丁二腈、2,3,3-三甲基丁二腈、2,2,3,3-四甲基丁二腈、2,3-二乙基-2,3-二甲基丁二腈、2,2-二乙基-3,3-二甲基丁二腈、双环己基-1,1-二腈、双环己基-2,2-二腈、双环己基-3,3-二腈、2,5-二甲基-2,5-己烷二腈、2,3-二异丁基-2,3-二甲基丁二腈、2,2-二异丁基-3,3-二甲基丁二腈、2-甲基戊二腈、2,3-二甲基戊二腈、2,4-二甲基戊二腈、2,2,3,3-四甲基戊二腈、2,2,4,4-四甲基戊二腈、2,2,3,4-四甲基戊二腈、2,3,3,4-四甲基戊二腈、马来腈、富马腈、1,4-二氰基戊烷、2,6-二氰基庚烷、2,7-二氰基辛烷、2,8-二氰基壬烷、1,6-二氰基癸烷、1,2-二氰基苯、1,3-二氰基苯、1,4-二氰基苯、3,3'-(亚乙基二氧基)二丙腈、3,3'-(亚乙二硫基)二丙腈、3,9-双(2-氰乙基)-2,4,8,10-四氧杂螺[5,5]十一烷等。
腈化合物优选为二腈化合物,更优选为由下式(4)表示的化合物,
【化学式3】
(式中,R5表示碳原子数1~6的烷基或碳原子数6~10的芳基)。
上述R5优选为碳原子数1~6的烷基。碳原子数1~6的烷基例如有:甲基、乙基、正丙基、异丙基、正丁基、叔丁基、正戊基、异戊基、正己基等。
二腈化合物优选为丙二腈、丁二腈、戊二腈、己二腈、庚二腈、辛二腈,更优选为丙二腈、丁二腈、戊二腈、己二腈。
羧酸酐例如有:琥珀酸酐、戊二酸酐、马来酸酐、柠康酸酐、戊烯二酸酐、衣康酸酐、二乙醇酸酐、环己烷二羧酸酐、环戊烷四羧酸二酐、苯基琥珀酸酐等。
硫酸酯化合物例如有甲磺酸甲酯、三亚甲基二醇硫酸酯等。
硫醚化合物例如有一硫化四甲基秋兰姆等。
亚硫酸酯化合物例如有亚硫酸乙烯酯等。
含氮化合物例如有:二甲基甲酰胺、二甲基乙酰胺等含氮链状化合物、1-甲基-2-吡咯烷酮、1-甲基-2-哌啶酮、3-甲基-2-噁唑烷酮、1,3-二甲基-2-咪唑啉酮、N-甲基琥珀酰亚胺等含氮环状化合物等。
盐解离剂更优选为丙二腈、丁二腈、戊二腈、己二腈、碳酸乙烯酯、碳酸丙烯酯、氟代乙烯碳酸酯、环丁砜、二甲基乙酰胺,进一步优选为丙二腈、丁二腈、戊二腈、碳酸乙烯酯、碳酸丙烯酯、二甲基乙酰胺,最优选为丁二腈、碳酸乙烯酯。
<聚合引发剂>
优选,本发明的电解质组合物含有聚合引发剂。聚合引发剂例如有光自由基聚合引发剂、热自由基聚合引发剂、阴离子聚合引发剂、阴离子光聚合引发剂、环氧树脂固化剂。光自由基聚合引发剂通过照射活性能量射线而能够产生聚合引发自由基;热自由基聚合引发剂通过加热而能够产生聚合引发自由基。阴离子光聚合引发剂通过照射活性能量射线而能够产生聚合引发阴离子种,从而能够引发聚合反应。环氧树脂固化剂在使环氧树脂固化时用作固化剂,能够引发环氧基的开环聚合反应。需要说明的是,此处所说的阴离子聚合引发剂是指引发产生聚合引发阴离子种的聚合反应的成分,不属于阴离子光聚合引发剂。
所述光自由基聚合引发剂没有特别限定,例如有:二乙氧基苯乙酮、2-羟基-2-甲基-1-苯基丙烷-1-酮、苄基二甲基缩酮、4-(2-羟基乙氧基)苯基-(2-羟基-2-丙基)酮、1-羟基环己基苯酮、2-甲基-2-吗啉代(4-硫代甲基苯基)丙烷-1-酮、2-苄基-2-二甲基氨基-1-(4-吗啉代苯基)丁酮、2-羟基-2-甲基-1-[4-(1-甲基乙烯基)苯基]丙酮低聚物、2,2-二甲氧基-1,2-二苯基乙烷-1-酮、1-[4-(2-羟基乙氧基)苯基]-2-羟基-2-甲基-1-丙烷-1-酮、2-羟基-1-{4-[4-(2-羟基-2-甲基丙酰基)苄基]苯基}-2-甲基丙烷-1-酮、2-二甲基氨基-2-[(4-甲基苯基)甲基]-1-[4-(4-吗啉基)苯基]-1-丁酮等苯乙酮类;苯甲酮、邻苯甲酰苯甲酸甲酯、4-苯基二苯甲酮、4-苯甲酰基-4'-甲基-二苯硫醚、3,3',4,4'-四(叔丁基过氧羰基)二苯甲酮、2,4,6-三甲基二苯甲酮、4-苯甲酰基-N,N-二甲基-N-[2-(1-氧代-2-丙烯氧基)乙基]苯甲基溴化铵、(4-苯甲酰基苄基)三甲氯化铵等二苯甲酮类;安息香、安息香甲醚、安息香乙醚、安息香异丙醚、安息香异丁醚等安息香类;2-异丙基噻吨酮、4-异丙基噻吨酮、2,4-二乙基噻吨酮、2,4-二氯噻吨酮、1-氯-4-丙氧基噻吨酮、2-(3-二甲基氨基-2-羟基)-3,4-二甲基-9H-噻吨酮-9-一氯甲烷等噻吨酮类;2,4,6-三甲基苯甲酰基二苯基氧化膦、双(2,4,6-三甲苯甲酰基)苯基氧化膦等酰基氧化膦类;双(η5-2,4-环戊二烯-1-基)-双(2,6-二氟-3-(1H-吡咯-1-基)苯基)钛等二茂钛类;1,2-辛二酮、1-[4-(苯硫基)-,2-(O-苯甲酰肟)]、乙酮、1-[9-乙基-6-(2-甲基苯甲酰基)-9H-咔唑-3-基]-,1-(O-乙酰肟)等肟酯类;氧基苯乙酸、2-[2-氧代-2-苯基乙酰氧基乙氧基]乙酯、氧基苯乙酸、2-(2-羟基乙氧基)乙酯等氧基苯乙酸酯类等。上述光自由基聚合引发剂可以单独使用,也可以两种以上同时使用。上述光自由基聚合引发剂中,优选为苯乙酮类、二苯甲酮类、酰基氧化膦类,特别优选为1-羟基环己基苯基酮、二苯甲酮、2-羟基-2-甲基-1-苯基丙烷-1-酮、2-甲基-2-吗啉代(4-硫代甲基苯基)丙烷-1-酮、1-[4-(2-羟基乙氧基)苯基]-2-羟基-2-甲基-1-丙烷-1-酮、2,4,6-三甲基苯甲酰基二苯基氧化膦。
所述热自由基聚合引发剂没有特别限定,例如有:过氧化甲乙酮、过氧化环己酮、过氧化甲基环己酮、过氧化乙酰乙酸甲酯、过氧化乙酰乙酸酯、1,1-双(叔己基过氧基)-3,3,5-三甲基环己烷、1,1-双(叔己基过氧基)-环己烷、1,1-双(叔丁基过氧基)-3,3,5-三甲基环己烷、1,1-双(叔丁基过氧基)-2-甲基环己烷、1,1-双(叔丁基过氧基)-环己烷、1,1-双(叔丁基过氧基)环十二烷、1,1-双(叔丁基过氧基)丁烷、2,2-双(4,4-二叔丁基过氧基环己基)丙烷、氢过氧化薄荷烷(p-menthane hydroperoxide)、氢过氧化二异丙苯(diisopropylbenzene hydroperoxide)、氢过氧化1,1,3,3-四甲基丁基酯(1,1,3,3-tetramethylbutyl hydroperoxide)、氢过氧化异丙苯(cumene hydroperoxide)、叔己基过氧化氢(t-hexyl hydroperoxide)、叔丁基过氧化氢(t-butyl hydroperoxide)、α,α’-双(叔丁基过氧基)二异丙苯、过氧化二异丙苯(dicumyl peroxide)、2,5-二甲基-2,5-双(叔丁基过氧基)己烷、过氧化叔丁基异丙苯(t-butylcumyl peroxide)、二叔丁基过氧化物、2,5-二甲基-2,5-双(叔丁基过氧基)己炔-3、过氧化异丁酰、3,5,5-三甲基己酰基过氧化物、过氧化辛酰、过氧化月桂酰、过氧化硬脂酰、过氧化琥珀酸、过氧化间甲苯酸酯(m-toluoyl peroxide)、过氧化苯甲酰、过氧化二碳酸二正丙酯、过氧化二碳酸二异丙酯、过氧化二碳酸双(4-叔丁基环己基)酯、过氧化二碳酸二-2-乙氧基乙酯、过氧化二碳酸二-2-乙氧基己酯、过氧化二碳酸二3-甲氧基丁酯、过氧化二碳酸二仲丁酯、过氧化二碳酸二(3-甲基-3-甲氧基丁基)酯、α,α’-双(新癸酰基过氧化)二异丙基苯(α,α'-bis(neodecanoylperoxy)diisopropylbenzene)、异丙苯基过氧化新癸酸酯(cumylperoxyneodecanoate)、过氧化新癸酸1,1,3,3-四甲基丁酯、过氧化新癸酸1-环己基-1-甲基乙酯、过氧化新癸酸叔己酯、过氧化新癸酸叔丁酯、过氧化新戊酸叔己酯、过氧化新戊酸叔丁酯、1,1,3,3-四甲基丁基过氧化-2-乙基己酸酯(1,1,3,3-tetramethylbutylperoxy-2-ethylhexanoate)、2,5-二甲基-2,5-双(2-乙基己酰基过氧化)己烷、1-环己基-1-甲基乙基过氧化-2-乙基己酸酯、叔己基过氧化-2-乙基己酸酯、叔丁基过氧化-2-乙基己酸酯、叔己基过氧化异丙基单碳酸酯、叔丁基过氧化异丁酸酯(t-butylperoxy isobutyrate)、叔丁过氧化马来酸酯(t-butyl peroxymalate)、叔丁基过氧化-3,5,5-三甲基己酸酯、过氧化月桂酸叔丁酯、叔丁基过氧化异丙基单碳酸酯(t-butylperoxyisopropyl monocarbonate)、叔丁基过氧化-2-乙基己基单碳酸酯(t-butylperoxy-2-ethylhexyl monocarbonate)、过氧化乙酸叔丁酯、叔丁基过氧化-间甲苯甲酰基苯甲酸酯、过氧化苯甲酸叔丁酯、双(叔丁基过氧化)间甲苯二酸酯(bis(t-butylperoxy)isophthalate)、2,5-二甲基-2,5-双(间甲苯甲酰基过氧化)己烷、过氧化苯甲酸叔己酯、2,5-二甲基-2,5-双(苯甲酰基过氧化)己烷、过氧化烯丙基单碳酸叔丁酯、叔丁基三甲基甲硅烷基过氧化物(t-butyltrimethylsilyl peroxide)、3,3’,4,4’-四(叔丁基过氧化羰基)苯甲酮(3,3',4,4'-tetra(t-butylperoxycarbonyl)benzophenone)、2,3-二甲基-2,3-二苯基丁烷等有机过氧化物系引发剂;
2-苯基偶氮-4-甲氧基-2,4-二甲基戊腈、1-[(1-氰基-1-甲基乙基)偶氮]甲酰胺、1,1’-偶氮双(环己烷-1-甲腈)、2,2’-偶氮双(2-甲基丁腈)、2,2’-偶氮双异丁腈、2,2’-偶氮双(2,4-二甲基戊腈)、2,2'-偶氮双(4-甲氧基-2,4-二甲基戊腈)、2,2'-偶氮双(2-甲基丙酰脒)二氢氯化物(2,2'-azobis(2-methylpropionamidine)dihydrochloride)、2,2’-偶氮双(2-甲基-N-苯基丙酰脒)二氢氯化物、2,2’-偶氮双[N-(4-氯苯基)-2-甲基丙酰脒)])二氢氯化物、2,2’-偶氮双[N-(4-氢苯基)-2-甲基丙酰脒)])二氢氯化物、2,2’-偶氮双[2-甲基-N-(苯基甲基)丙酰脒])二氢氯化物、2,2’-偶氮双[2-甲基-N-(2-丙烯基)丙酰脒]二氢氯化物、2,2’-偶氮双[N-(2-羟基乙基)-2-甲基丙酰脒)]二氢氯化物、2,2’-偶氮双[2-(5-甲基-2-咪唑啉-2-基)丙烷]二氢氯化物、2,2’-偶氮双[2-(2-咪唑啉-2-基)丙烷]二氢氯化物、2,2’-偶氮双[2-(4,5,6,7-四氢-1H-1,3-二氮杂卓-2-基)丙烷]二氢氯化物(2,2'-azobis[2-(4,5,6,7-tetrahydro-1H-1,3-diazepine-2-yl)propane)dihydrochloride)、2,2’-偶氮双[2-(3,4,5,6-四氢嘧啶-2-基)丙烷]二氢氯化物、2,2’-偶氮双[2-(5-羟基-3,4,5,6-四氢嘧啶-2-基)丙烷]二氢氯化物、2,2’-偶氮双{2-[1-(2-羟基乙基)-2-咪唑啉-2-基]丙烷}二氢氯化物、2,2’-偶氮双[2-(2-咪唑啉-2-基)丙烷]、2,2’-偶氮双{2-甲基-N-[1,1-双(羟基甲基)-2-羟基乙基]丙酰胺}、2,2’-偶氮双{2-甲基-N-[1,1-双(羟基甲基)乙基]丙酰胺}、2,2’-偶氮双[2-甲基-N-(2-羟基乙基)丙酰胺]、2,2’-偶氮双(2-甲基丙酰胺)、2,2’-偶氮双(2,4,4-三甲基戊烷)、2,2’-偶氮双(2-甲基丙烷)、二甲基-2,2-偶氮双(2-甲基丙酸酯)、4,4’-偶氮双(4-氰基戊烷酸)、2,2’-偶氮双[2-(羟基甲基)丙腈]等偶氮系引发剂;
二乙氧基苯乙酮、2-羟基-2-甲基-1-苯基丙烷-1-酮、苄基二甲基缩酮、4-(2-羟基乙氧基)苯基-(2-羟基-2-丙基)酮、1-羟基环己基苯基酮、2-甲基-2-吗啉代(4-硫代甲基苯基)丙烷-1-酮、2-苄基-2-二甲基氨基-1-(4-吗啉代苯基)丁酮、2-羟基-2-甲基-1-[4-(1-甲基乙烯基)苯基]丙酮低聚物等苯乙酮类;安息香、安息香甲醚、安息香乙醚、安息香异丙醚、安息香异丁醚等安息香类;二苯甲酮、苯甲酸邻苯甲酰基甲酯(o-benzoyl methyl benzoate)、4-苯基二苯甲酮、4-苯甲酰基-4'-甲基-二苯硫醚、3,3',4,4'-四(叔丁基过氧羰基)二苯甲酮、2,4,6-三甲基二苯甲酮、4-苯甲酰基-N,N-二甲基-N-[2-(1-氧代-2-丙烯氧基)乙基]苯溴化甲酰胺盐(4-benzoyl-N,N-dimethyl-N-[2-(1-oxo-2-propenyloxy)ethyl]benzene methanaminiumbromide)、(4-苯甲酰基苄基)三甲氯化铵等二苯甲酮类;2-异丙基噻吨酮、4-异丙基噻吨酮、2,4-二乙基噻吨酮、2,4-二氯噻吨酮、1-氯-4-丙氧基噻吨酮、2-(3-二甲基胺基-2-羟基)-3,4-二甲基-9H-噻吨酮-9-酮间甲烷(2-(3-dimethylamino-2-hydroxy)-3,4-dimethyl-9H-thioxanthone-9-one methochloride)等噻吨酮类;等。上述自由基聚合热引发剂可以单独使用,也可以两种以上同时使用。上述热自由基聚合引发剂中,优选为有机过氧化物系引发剂、偶氮系引发剂。
所述阴离子聚合引发剂没有特别限定,例如有:萘钠、正丁基锂、叔丁基锂等具有碱金属和碳阴离子的碱金属化合物;三甲基铝、三乙基铝、三丙基铝、三异丙基铝、三丁基铝、三异丁基铝等三烷基铝类;氯二烷基铝、氯二乙基铝、氯二丙基铝、氯二异丙基铝、氯二丁基铝、氯二异丁基铝、双(五甲基环戊烯)钐、甲基-双(五甲基环戊烯)钐等。
所述阴离子光聚合引发剂没有特别限定,例如有烷氧基钛、对氯苯基-邻硝基苄基醚等。
上述阴离子聚合引发剂和/或阴离子光聚合引发剂可以分别单独使用或两种以上同时使用。
所述环氧树脂固化剂没有特别限定,例如有:二亚乙基三胺、三亚乙基四胺、二丙烯二胺等链状脂肪族多胺类;N-氨基乙基哌嗪、薄荷烷二胺、异佛尔酮二胺等环状脂肪族多胺类;间苯二胺、二氨基二苯基甲烷等芳香族胺类;1,8-二氮杂二环(5,4,0)-十一碳烯-7、1,5-二氮杂二环(4,3,0)-壬烯-5、三(二甲基氨基甲基)苯酚等叔胺类;1-氰乙基-2-乙基-4-甲基咪唑、2-乙基-4-甲基咪唑等咪唑类;乙二醇双偏苯三酸酐(ethylene glycol bis(trimellitate)、四氢邻苯二甲酸酐、琥珀酸酐、甲基环己烯二羧酸酐、次氯酸酐、聚(壬二酸酐)、4-甲基六氢邻苯二甲酸酐等酸酐类;二苯基碘鎓六氟磷酸盐、三苯基锍六氟磷酸盐等阳离子聚合光引发剂;双氰胺、三苯基膦、四苯基鏻/四苯基硼酸盐等。上述环氧树脂固化剂可以单独使用,也可以两种以上同时使用。
<其他成分>
本发明的电解质组合物也可以含有碱金属盐、光固化单体和/或热固化单体、盐解离剂、聚合引发剂以外的其他成分。其他成分例如有:聚醚系聚合物、(甲基)丙烯酸系聚合物、腈系聚合物、氟系聚合物等聚合物;庚烷、辛烷、环庚烷等饱和烃化合物;乙腈、丙腈、丁腈、戊腈、碳酸二甲酯(DMC)、碳酸二乙酯(DEC)、碳酸甲乙酯(EMC)、磺酸内酯等有机溶剂;等。
所述其他成分的含量相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总含量100质量%优选在30质量%以下,更优选在25质量%以下,进一步优选在20质量%以下。
[电解质膜]
本发明还是一种将所述电解质组合物固化而得到的电解质膜。
本发明又是一种将电解质组合物用作电解质膜的原料的方法。
本发明的电解质组合物因为制膜性优异,所以不使用支承体(隔膜)就能够形成电解质膜,即能够形成自支撑膜。
本发明的电解质膜优选为不包括支承体的自支撑膜,但也可以包括支承体。
所述支承体(隔膜)没有特别限制,例如有:机织布、无纺布、(微)多孔膜以及玻璃成型体等。
所述机织布和无纺布例如由下述物质形成,它们是聚丙烯、聚乙烯、聚甲基戊烯等聚烯烃系树脂、聚对苯二甲酸乙二醇酯(PET)等聚酯系树脂、尼龙等聚酰胺系树脂、聚对苯二甲酰对苯二胺等芳香族聚酰胺系树脂、丙烯酸系树脂、聚乙烯醇系树脂、纤维素系树脂(纤维素系纤维)等;氧化铝纤维、陶瓷纤维、玻璃纤维等。
所述(微)多孔膜例如由下述物质形成,它们是聚丙烯、聚乙烯、乙烯-丙烯共聚物等聚烯烃系树脂、聚酯系树脂、四氟乙烯-全氟烷氧基乙烯共聚物等氟树脂、聚醚醚酮、聚对苯二甲酸丁二醇酯、聚苯硫醚、聚酰胺系树脂、聚酰亚胺等。
所述玻璃成型体例如有玻璃布。
为了进一步提高亲水性,上述隔膜可以通过添加表面活性剂的方法、利用发烟硫酸、氯磺酸等化学品进行磺化、氟化、接枝处理等的方法或电晕放电、等离子体放电等方法进行亲水化处理。
所述隔膜优选由下述物质形成,它们是选自由纤维素无纺布、PET无纺布、玻璃无纺布、聚烯烃无纺布、聚烯烃微多孔膜以及聚酰亚胺多孔膜组成的群组的至少一种。更优选为纤维素无纺布、聚烯烃微多孔膜。
所述电解质膜的膜厚优选为5~300μm。更优选为10~250μm,进一步优选为15~200μm。
[电解质膜的制造方法]
在将本发明的电解质组合物固化而得到电解质膜时,可以使用沸点低于盐解离剂的有机溶剂,但在能够使所述电解质组合物中的碱金属盐和盐解离剂溶于光固化单体和/或热固化单体时或能够使光固化单体和/或热固化单体、碱金属盐溶于盐解离剂时,不使用所述有机溶剂也能够得到电解质膜,从安全性、环境的观点出发,不使用所述有机溶剂为优选。
本发明还是一种电解质膜的制造方法,所述制造方法也是下述电解质膜的制造方法,包括将所述电解质组合物固化的工序,所述固化工序中,沸点低于盐解离剂的有机溶剂的用量相对于所述组合物中的碱金属盐、光固化单体和/或热固化单体、盐解离剂的总含量100质量%在20质量%以下。
本发明也是一种电解质膜,通过将所述电解质组合物固化而得到,所述电解质组合物中的沸点低于盐解离剂的有机溶剂的含量相对于碱金属盐、具有源自于光固化单体和/或热固化单体的结构单元的聚合物、盐解离剂的总含量100质量%在20质量%。
在所述固化工序中,沸点低于盐解离剂的有机溶剂的用量和有机溶剂在所述电解质组合物中的含量优选在18质量%以下,更优选在15质量%以下,进一步优选在12质量%以下,特别优选在10质量%以下。
所述有机溶剂只要沸点低于盐解离剂便没有特别限制,优选为可将碱金属盐、光固化单体和/或热固化单体以及盐解离剂均匀溶解的溶剂。
有机溶剂的具体例优选为乙腈、碳酸二甲酯、碳酸甲乙酯。
此外,有机溶剂与盐解离剂的沸点差,优选在摄氏50℃以上,更优选在摄氏80℃以上,最优选在摄氏100℃以上。如果沸点差在上述优选范围内,则能充分抑制有机溶剂干燥时盐解离剂减少,从而能够更充分地发挥本发明的作用和效果。
所述有机溶剂的沸点优选在摄氏150℃以下,更优选在摄氏120℃以下。
[电池材料]
本发明的电解质组合物非常适合用作电解质膜、电极等各种电池材料。
像这样,使用本发明的电解质组合物的电池材料也是本发明的一个方面。
<电极>
本发明的电解质组合物适合用作电池所使用的电极的材料。
由本发明的电解质组合物形成的电极也是本发明的一个方面。本发明的电解质组合物可以用于正极,也可以用于负极。
正极是由正极集电体承载含有正极活性物质、导电助剂、粘结剂以及分散溶剂等的正极活性物质组合物而形成的,通常成型为片状。
正极的制造方法例如有:通过刮刀法将正极活性物质组合物涂布到正极集电体上,将正极集电体浸渍于正极活性物质组合物中之后再干燥的方法;将正极活性物质组合物混炼成型并干燥而得到片材,将片材通过导电性粘合剂粘接到正极集电体上后,压制、干燥的方法;将添加有液状润滑剂的正极活性物质组合物涂布或流延到正极集电体上,成型为期望的形状后,除去液状润滑剂,然后沿单轴或多轴延伸的方法;等。
正极集电体的材料没有特别限定,例如能够使用铝、铝合金、SUS(不锈钢)、钛等导电性金属。从容易加工成薄膜且廉价的观点出发,优选为其中的铝。
正极活性物质只要能储存、释放离子即可,能够使用现有公知的正极活性物质。具体而言,正极活性物质例如有MCoO2、MNiO2、MMnO2、由MNi1-x-yCoxMnyO2、MNi1-x-yCoxAlyO2(0≤x≤1,0≤y≤1)表示的三元系氧化物等过渡金属氧化物、由MxNiyMn(2-y)O4(0.9≤x≤1.1,0<y<1)表示的镍锰酸、MAPO4(A=Fe、Mn、Ni、Co)等具有橄榄石结构的化合物、加入多种过渡金属的固溶材料(电化学惰性的层状M2MnO3和电化学活性的层状MM”O([M”=Co、Ni等过渡金属]的固溶体)(M表示碱金属离子)等。上述正极活性物质可以单独使用一种,也可以多种组合使用。
导电助剂例如有乙炔炭黑、炭黑、石墨、金属粉末材料、单层碳纳米管、多层碳纳米管、气相生长炭纤维等。
粘结剂例如有:聚偏氟乙烯、聚四氟乙烯等氟系树脂;苯乙烯-丁二烯橡胶、腈丁二烯橡胶等合成橡胶;聚酰胺酰亚胺等聚酰胺系树脂;聚乙烯、聚丙烯等聚烯烃系树脂;聚(甲基)丙烯酸系树脂;聚丙烯酸;羧甲基纤维素等纤维素系树脂;等。上述粘结剂可以单独使用,也可以多种组合使用。此外,上述粘结剂在使用时可以是溶解于溶剂中的状态,也可以是分散于溶剂中的状态。
导电助剂和粘结剂的添加量能够考虑着电池的使用目的(重视输出、重视能量等)、离子电导性等适当地进行调节。
制造正极时,用于正极活性物质组合物的溶剂例如有N-甲基吡咯烷酮、二甲基甲酰胺、二甲基乙酰胺、甲基乙基甲酮、四氢呋喃、乙腈、丙酮、乙醇、乙酸乙酯、水等。上述溶剂可以组合使用。溶剂的用量没有特别限定,只要根据制造方法、使用的材料适当决定即可。
负极活性物质能够采用电池所使用的现有公知的负极活性物质,只要能储存、释放离子即可。具体而言,能够采用碱金属、碱金属-铝合金等金属合金、人造石墨、天然石墨等石墨材料、用煤炭、石油沥青制成的中间相烧结体、难石墨化碳等碳材料、Si、Si合金、SiO等Si系负极材料、Sn合金等Sn系负极材料。
负极的制造方法能够采用与正极的制造方法相同的方法。此外,制造负极时使用的导电助剂、粘结剂、用于分散材料的溶剂也都能够采用与制造正极时相同的物质。
本发明的电解质组合物可以与作为粘合剂的正极或负极材料浆料混合后涂布到基板上,也可以将正极或负极材料浆料涂布到基板上并干燥后,进一步涂布含有本发明的电解质组合物的电解质溶液并干燥。
所述电解质除了本发明的电解质组合物以外,能够同时使用高分子固体电解质、无机固体电解质、熔融盐等。优选使用本发明的电解质组合物。
<电池>
本发明也是一种使用本发明的电解质膜和/或电极构成的电池。
本发明的电池优选包括上述本发明的电解质膜作为隔膜。更详细而言,优选地,本发明的电池是包括正极和负极的二次电池,在正极与负极之间设有电解质膜,与正极、负极等一起收纳在外壳中。
本发明所涉及的电池的形状没有特别限定,电池的形状能够采用圆柱形、方形、层叠型、硬币型、大型等现有公知的任何形状。此外,在本发明所涉及的电池用作搭载到电动汽车、混合动力电动汽车等上的高电压电源(几十V~几百V)的情况下,还能够使本发明所涉及的电池成为将各个电池串联而成的电池模组。
所述电池优选为碱金属电池,使用本发明的电解质膜和/或电极构成的碱金属电池也是本发明的一方面。此外,本发明的一个优选实施方式是,由上述本发明的电解质组合物形成的电解质膜或电极是碱金属电池用电解质膜或电极。
所述电池更优选为二次电池,本发明的一个优选实施方式是,所述电池是锂离子二次电池。
【实施例】
下面举出实施例对本发明进行更详细的说明,但本发明不限于以下实施例。需要说明的是,只要没有特别说明,“份”均指“重量份”,“%”均指“质量%”,“Mw”均指“重均分子量”。此外,有时将“升”记作“L”,将“摩尔/升”记作“M”。
<合成例1>含交联基的聚环氧烷共聚物的合成
将包括搅拌机、添加口以及温度传感器的1L高压釜反应器用氮气置换后,依次加入用分子筛进行脱水处理后的甲苯286.5份、叔丁氧基钾(1.0M四氢呋喃溶液)0.85份,用氮气加压,直至反应器内的压力达到表压0.3Mpa为止。
利用油浴使反应器的内温升高到90℃后,以0.85份/分的供给速度开始供给环氧乙烷,从开始供给环氧乙烷起经过30分后,以0.131份/分的供给速度开始供给单体混合物(重量比:环氧丁烷/烯丙基缩水甘油醚=8/3)。从开始供给环氧乙烷起经过2.5小时后,使供给速度分别降低到0.43份/分、0.053份/分,并定量供给5小时(环氧乙烷的供给量:共255份,单体混合物的供给量:共31.5份)。供给过程中,一边对由聚合热引起的内温上升和内压上升进行监控,一边在100℃±5℃下进行反应。供给结束后,在100℃±5℃下保持2小时,使之熟化。熟化结束后,通过减压脱挥从反应混合物中蒸馏除去溶剂,得到Mw为10.4万的含交联基的聚环氧烷共聚物(A)。
<合成例2>聚环氧乙烷聚合物(B)的合成
将包括搅拌机、添加口以及温度传感器的1L高压釜反应器用氮气置换后,依次加入用分子筛进行脱水处理后的甲苯335.3份、叔丁氧基钾(1.0M四氢呋喃溶液)1.61份,用氮气加压,直至反应器内的压力达到表压0.3MPa。
利用油浴使反应器的内温升高到95℃后,以1.12份/分的供给速度开始供给环氧乙烷,一边对聚合热引起的内温上升和内压上升进行监控一边适当地调节供给速度,在100℃±5℃下耗时350分连续供给环氧乙烷223.6份。供给结束后,在100℃±5℃下保持2小时,使之熟化。熟化结束后,通过减压脱挥从反应混合物中蒸馏除去溶剂,得到Mw11万的聚环氧乙烷聚合物(B)。
<实施例1-1>电解质膜(1)的制造
取1.4g的双(氟磺酰)亚胺锂(以下记作LiFSI)(NIPPON SHOKUBAI CO.,LTD.制造)、0.46g的固化单体(A)(SHIN-NAKAMURA CHEMICAL CO,LTD.制造,化学名(聚乙二醇#600二丙烯酸酯))、0.12g的碳酸乙烯酯(LBG级,KISHIDA CHEMICAL Co.,Ltd.制造)作为电解质盐,与0.02g的聚合引发剂(ESACURE KTO46(2,4,6-三甲基苯甲酰基二苯基氧化膦、α-羟基酮以及二苯甲酮衍生物的混合物),DKSH Japan株式会社制造)一起称量到PP管瓶(10mL)中,用恒温槽以75℃加热60分钟使其溶解,得到期望的溶液(电解质溶液)。将制备出的电解质溶液涂布到特氟龙(注册商标)片上后,取50μm的PET薄膜用作隔膜,将特氟龙(注册商标)片覆盖在上表面上,并用平行平板压力机压平。隔着特氟龙(注册商标)片,用超高压水银灯(透射特氟龙(注册商标)片后为4.2mW/cm2(365nm))从两面各照射UV光60秒来进行光聚合反应,得到了膜厚48μm的电解质膜。
<实施例1-2>电解质膜(2)的制造
使添加比为1.3g的LiFSI、0.5g的固化单体(A)、0.18g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚44μm的电解质膜。
<实施例1-3>电解质膜(3)的制造
使添加比为1.3g的LiFSI、0.54g的固化单体(C)(SHIN-NAKAMURA CHEMICAL CO,LTD.制造,化学名(聚乙二醇#1000二丙烯酸酯))、0.14g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚50μm的电解质膜。
<实施例1-4>电解质膜(4)的制造
使添加比为1.3g的LiFSI、0.38g的固化单体(A)、0.12g的固化单体(B)(SHIN-NAKAMURA CHEMICAL CO,LTD.制造,化学名(甲氧基聚乙二醇#600丙烯酸酯))、0.18g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚42μm的电解质膜。
<实施例1-5>电解质膜(5)的制造
使添加比为1.3g的LiFSI、0.5g的固化单体(A)、0.18g的丁二腈,其他方面与实施例1-1相同,这样得到了膜厚45μm的电解质膜。
<实施例1-6>电解质膜(6)的制造
使添加比为1.2g的LiFSI、0.6g的固化单体(A)、0.18g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚51μm的电解质膜。
<实施例1-7>电解质膜(7)的制造
使添加比为1.2g的LiFSI、0.5g的固化单体(A)、0.28g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚45μm的电解质膜。
<实施例1-8>电解质膜(8)的制造
使添加比为1.1g的LiFSI、0.6g的固化单体(A)、0.28g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚49μm的电解质膜。
<实施例1-9>电解质膜(9)的制造
使添加比为1.0g的LiFSI、0.7g的固化单体(A)、0.28g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚56μm的电解质膜。
<实施例1-10>电解质膜(10)的制造
使添加比为1.3g的LiFSI、0.5g的固化单体(C)(SHIN-NAKAMURA CHEMICAL CO,LTD.制造,化学名(聚乙二醇#1000二丙烯酸酯))、0.18g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚32μm的电解质膜。
<实施例1-11>电解质膜(11)的制造
使添加比为1.3g的LiFSI、0.44g的固化单体(C)(SHIN-NAKAMURA CHEMICAL CO,LTD.制造,化学名(聚乙二醇#1000二丙烯酸酯))、0.24g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚37μm的电解质膜。
<实施例1-12>电解质膜(12)的制造
使添加比为1.2g的LiFSI、0.12g的乙腈(LBG级,KISHIDA CHEMICAL Co.,Ltd.制造)(溶剂A)、0.44g的固化单体(A)、0.22g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚58μm的电解质膜。
<实施例1-13>电解质膜(13)的制造
使添加比为1.3g的LiFSI、0.12g的乙腈(LBG级,KISHIDA CHEMICAL Co.,Ltd.制造)(溶剂A)、0.32g的固化单体(A)、0.24g的碳酸乙烯酯、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚56μm的电解质膜。
<实施例1-14>电解质膜(14)的制造
使添加比为1.3g的LiFSI、0.4g的固化单体(B)、0.28g的二甲基砜(特级试剂,FUJIFILM Wako Pure Chemical Corporation制造)、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚52μm的电解质膜。
<实施例1-15>电解质膜(15)的制造
使添加比为1.3g的LiFSI、0.4g的固化单体(B)、0.4g的固化单体(D)(SHIN-NAKAMURA CHEMICAL CO,LTD.制造,商品名(UA-7100,聚氨酯丙烯酸酯)、0.14g的二甲基砜、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚52μm的电解质膜。
<实施例1-16>电解质膜(16)的制造
使添加比为1.2g的LiTFSI(LBG级,KISHIDA CHEMICAL Co.,Ltd.制造)、0.46g的固化单体(B)、0.32g的二甲基砜、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚55μm的电解质膜。
<实施例1-17>电解质膜(17)的制造
使添加比为1.3g的LiTFSI、0.2g的固化单体(B)、0.2g的固化单体(D)、0.28g的二甲基砜、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚55μm的电解质膜。
<实施例1-18>电解质膜(18)的制造
使添加比为1.1g的LiFSI、0.2g的LiTFSI、0.2g的固化单体(B)、0.2g的固化单体(D)、0.28g的二甲基砜、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚60μm的电解质膜。
<比较例1-1>比较电解质膜(1)的制造
将0.2g的LiTFSI、0.79g的聚合物(A)、0.01g的聚合引发剂称量到PP管瓶(10mL)中,混合溶解1.6mL的乙腈(LBG级,KISHIDA CHEMICAL Co.,Ltd.制造),得到电解质溶液。将制备出的电解质溶液涂布到特氟龙(注册商标)片上后,用热风干燥机以40℃进行30分钟的加热干燥后,用减压干燥机以绝对压力为真空度-0.1MPa、40℃下进行24小时的减压干燥,由此除去溶剂。将特氟龙(注册商标)片覆盖在干燥后的膜上表面后,用超高压水银灯(透射特氟龙(注册商标)片后为4.2mW/cm2(365nm))从两面各照射UV光60秒来进行光聚合反应,得到了膜厚28μm的电解质膜。
<比较例1-2>比较电解质膜(2)的制造
使添加比为0.12g的LiFSI、0.87g的聚合物(A)、0.01g的聚合引发剂,其他方面与比较例1-1相同,这样得到了膜厚30μm的电解质膜。
<比较例1-3>比较电解质膜(3)的制造
使添加比为1.3g的LiFSI、0.68g的固化单体(A)、0.02g的聚合引发剂,其他方面与实施例1-1相同,这样得到了膜厚50μm的电解质膜。
将实施例1-1~1-11和比较例1-1~1-3中使用的各成分的添加量示于表1,将实施例1-12~1-18中使用的各成分的添加量示于表2。
【表1】
【表2】
<离子电导率和锂迁移数测量>
使用多通道电化学工作站(VSP-300,Biologic公司制造)测量离子电导率和锂迁移数。用的冲头对实施例1-1~1-11和比较例1-1~1-3中制备的电解质膜进行冲裁而得到片材,用两张的锂箔(0.2mm厚,Honjo Metal Co.,Ltd.制造)夹住该片材后,用两片SUS316L制隔膜(0.5mm厚,Hohsen Corp.制造)进一步夹住而固定到测量装置的夹具上。在温度40℃的环境下,以电流值IS=+0.0785mA(0.1mA/cm2)进行1分的通电处理,以IS=-0.0785mA进行1分的通电处理,上述处理重复五次。使用同一装置,在1MHz~10mHz、振幅10mV的条件下进行阻抗分析,将从Cole-cole图得到的体电阻分量设为Rb,将锂箔与电解质膜的界面电阻分量设为RSi(Ω)。然后,进行20mV的电压施加试验5分钟,刚施加电压后的电流值与5分后的电流值分别设为Ii(A)、Ic(A)。在施加有20mV电压的状态下,在1MHz~10mHz、振幅10mV的条件下进行阻抗分析,将从Cole-cole图得到的锂箔与电解质膜的界面电阻分量设为RSc(Ω)。将测量试样的厚度设为T(cm),将电解质膜与锂箔的接触面积设为测量试样的面积A(cm2),根据下式(α)计算离子电导率σ(S/cm)。
σ=T/A/Rb(α)
设施加电压为E(V),根据下式(β)计算锂迁移数。
tLi=Ic(E-RSiIi)/Ii(E-RScIc)(β)
将结果示于表3。
<锂离子电导性评价(通电负荷试验)>
下面,以I=±0.157mA(±0.2mA/cm2)进行各3分钟的通电试验,以I=±0.236mA(±0.3mA/cm2)进行各3分钟的通电试验,以I=±0.314mA(±0.4mA/cm2)进行各3分钟的通电试验,以I=±0.393mA(±0.5mA/cm2)进行各3分钟的通电试验,以I=±0.471mA(±0.6mA/cm2)进行各3分钟的通电试验,然后使施加的电流值以0.2mA/cm2为单位持续上升。随着电流值上升,电解质膜上的负荷会上升,因此在某电流值以上时,锂离子无法导电,通电时电动势达到1.5V。根据连续通电3分钟后达到1.5V时的电流值,判断锂离子的易流动度。将结果示于表3。
【表3】
表3的结果表明,本发明得到的实施例1-1~1-18的电解质膜虽然离子电导率与比较例1-1~1-2相比显示出较低的值,但具有较高的锂迁移数,结果在通电负荷试验中具有优异的离子电导性。表3的结果还表明,与比较例1-3相比,本发明得到的实施例1-1~1-18的电解质膜通过添加盐解离剂,能够实现优异的离子电导性。
<实施例2-1>锂离子二次电池(1)的制备
取LiNi1/3Co1/3Mn1/3O2(Umicore制造)100份作为正极活性物质,取乙炔炭黑(粉状品,Denka Company Limited制造)3份、石墨粉末(J-SP,Nippon Graphite Industries,Co.,Ltd.制造)3份作为导电助剂,取聚偏氟乙烯(#7200,KUREHA CORPORATION制造)3份作为粘结剂,将上述物质分散到N-甲基吡咯烷酮(LBG级,KISHIDA CHEMICAL Co.,Ltd.制造)中而得到正极合剂浆料。正极集电体采用铝箔(1085级材料),将所述正极浆料均匀涂布到铝箔上后,用热风干燥机以70℃进行30分钟的加热干燥,并用减压干燥机以绝对压力为真空度-0.1MPa、110℃下进行2小时的减压干燥来除去溶剂,得到正极重量9.8mg/cm2、膜厚35μm(不含铝箔)的正极片。
将实施例1-3制备的电解质溶液涂布到所述正极片上后,取50μm的PET薄膜用作隔膜,在上表面覆盖特氟龙(注册商标)片,并用平行平板压力机压平。隔着特氟龙(注册商标)片,用超高压水银灯(透射特氟龙(注册商标)片后4.2mW/cm2(365nm))照射UV光60秒来进行光聚合反应,制备出63μm厚(不含正极活性物质层的厚度)的涂布有电解质层的电解质膜一体化正极。
以对得到的电解质膜一体化正极进行冲裁而得到片材,将该片材用作电池的正极,将以冲裁后的0.5mm厚的锂箔用作负极,并以锂箔与电解质面相对的方式重叠。通过硬币型电池自动铆接机(Hohsen Corp.制造)将CR2032型硬币型电池部件(Hohsen Corp.制造)的正极壳、负极帽、1.0mm厚的SUS制隔膜、波形垫圈、垫片进行铆接,由此制备出硬币型锂离子二次电池。
<实施例2-2>锂离子二次电池(2)的制备
除了将实施例1-4制备的电解质溶液涂布到在所述正极片上以外,其他方面与实施例2-1相同,由此制备出71μm厚(不含正极活性物质层的厚度)的一体化正极,并制备出使用该一体化正极的锂离子二次电池。
<比较例2-1>比较锂离子二次电池(1)的制备
将0.2g的LiTFSI、0.8g的聚合物(B)以及1.6mL的乙腈混合溶解而得到电解质溶液。与实施例2-1同样地制备出正极片,将电解质溶液均匀涂布到该正极片上后,用热风干燥机以40℃进行30分钟的加热干燥,并用减压干燥机以绝对压力为真空度-0.1MPa、70℃下进行2小时的减压干燥来除去溶剂,得到含浸有锂盐和聚合物的复合正极片。
以对得到的复合正极片进行冲裁而得到片材,将该片材用作电池的正极,以对比较例1-1制备的电解质膜进行冲裁而得到片材,将该片材用作电解质膜,将以冲裁后的0.5mm厚的锂箔用作负极,以锂箔与正极的电解质涂布面相对的方式依次将锂箔、电解质膜、正极重叠。通过硬币型电池自动铆接机(Hohsen Corp.制造)将CR2032型硬币型电池部件(Hohsen Corp.制造)的正极壳、负极帽、1.0mm厚的SUS制隔膜、波形垫圈、垫片进行铆接,由此制备出硬币型锂离子二次电池。
<锂离子二次电池评价>
用充放电试验装置(ACD-01,ASKA ELECTRONIC CO.,LTD.制造)对实施例2-1、2-2和比较例2-1中得到的硬币型锂离子二次电池进行充放电试验。在温度40℃的环境下,在充电条件C/24(当正极容量为150mAh/g时,1小时充满电的电流值为1C)下充电至4.2V后,停止15分钟,再以放电条件C/24放电至2.5V。接着,以充电条件C/24充电至4.2V后,停止15分钟,再以放电条件C/6放电至2.5V,得到此时的放电曲线和放电容量。将得到的放电曲线示于图1。
图1表明,使用了由本发明的电解质组合物得到的电解质膜的锂离子二次电池(实施例2-1、2-2)与比较例2-1相比,能够得到较高的放电电压和较高的放电容量。
Claims (12)
1.一种电解质组合物,含有碱金属盐,其特征在于:该组合物还含有光固化单体和/或热固化单体、盐解离剂,碱金属盐的含量比例相对于碱金属盐、光固化单体和/或热固化单体、盐解离剂的总量100质量%在50质量%以上。
2.根据权利要求1所述的电解质组合物,其特征在于:
所述碱金属盐由下式(1)表示,
MN(SO2R1)(SO2R2) (1)
式中,M表示碱金属离子;R1、R2相同或不同,表示氟原子或碳原子数1~3的氟烷基。
3.根据权利要求1或2所述的电解质组合物,其特征在于:
所述碱金属盐是双氟磺酰亚胺的碱金属盐。
4.根据权利要求1到3中任一项权利要求所述的电解质组合物,其特征在于:
所述光固化单体和/或热固化单体具有杂元素。
5.根据权利要求1到4中任一项权利要求所述的电解质组合物,其特征在于:
所述光固化单体和/或热固化单体中含有多官能单体。
6.根据权利要求1到5中任一项权利要求所述的电解质组合物,其特征在于:
所述盐解离剂是碳酸酯化合物。
7.根据权利要求1到6中任一项权利要求所述的电解质组合物,其特征在于:
所述盐解离剂是磺酰基化合物。
8.根据权利要求1到7中任一项权利要求所述的电解质组合物,其特征在于:
所述盐解离剂是腈化合物。
9.根据权利要求1到8中任一项权利要求所述的电解质组合物,其特征在于:
所述电解质组合物含有聚合引发剂。
10.一种电解质膜,通过将权利要求1到9中任一项权利要求所述的电解质组合物固化而得到,其特征在于:
该电解质膜中含有碱金属盐、聚合物以及盐解离剂,所述聚合物具有源自于光固化单体和/或热固化单体的结构单元。
11.根据权利要求10所述的电解质膜,其特征在于:
该电解质膜也可以含有沸点低于所述盐解离剂的有机溶剂,该有机溶剂的含量相对于碱金属盐、聚合物、盐解离剂的总含量100质量%在20质量%以下,该聚合物具有源自于光固化单体和/或热固化单体的结构单元。
12.一种电解质膜的制造方法,其特征在于:该制造方法包括将权利要求1到9中任一项权利要求所述的电解质组合物固化的工序,在该固化工序中,沸点低于盐解离剂的有机溶剂的用量相对于该组合物中的碱金属盐、光固化单体和/或热固化单体、盐解离剂的总含量100质量%在20质量%以下。
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