CN1220030A - 适合作为电化学电池的固体电解质或隔板的组合物 - Google Patents
适合作为电化学电池的固体电解质或隔板的组合物 Download PDFInfo
- Publication number
- CN1220030A CN1220030A CN97194945A CN97194945A CN1220030A CN 1220030 A CN1220030 A CN 1220030A CN 97194945 A CN97194945 A CN 97194945A CN 97194945 A CN97194945 A CN 97194945A CN 1220030 A CN1220030 A CN 1220030A
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- acid
- carboxylic acid
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- 239000005054 phenyltrichlorosilane Substances 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
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- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
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- MSVPBWBOFXVAJF-UHFFFAOYSA-N tetradecane-1,14-diamine Chemical class NCCCCCCCCCCCCCCN MSVPBWBOFXVAJF-UHFFFAOYSA-N 0.000 description 1
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- 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
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- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Substances C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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Abstract
本发明涉及一种混合物Ⅰa,该混合物包括由以下组分组成的组合物Ⅱa: a)1-95%(重量)的固体物质Ⅲ,优选为碱性固体物质Ⅲ,具有主要粒度为5nm-20μm,和b)5-99%(重量)的通过聚合b1)和b2)所获得的聚合物Ⅳ:b1)按物质Ⅳ计,5-100%(重量)的以下组分的缩合产物Ⅴα)至少一种能够与羧酸或磺酸或其衍生物或其两种或多种的混合物反应的化合物Ⅵ,和β)对于每摩尔化合物Ⅵ而言至少1摩尔的具有至少一个可自由基聚合的官能团的羧酸或磺酸Ⅶ,或其衍生物或其两种或多种的组合物和b2)按物质Ⅳ计,0-95%(重量)的具有平均分子量(均数)为至少5000和在主链或侧链上具有聚醚链段的其它化合物Ⅷ,其中混合物Ⅰa中组合物Ⅱa的重量比例是1-100%(重量)。
Description
本发明涉及一种适合用于例如含有含锂电解质的电化学电池的混合物;其在例如固体电解质、隔板和电极中的应用;含有该混合物的固体电解质,隔板,电极,传感器,电致变色显示窗,显示器,电容器和离子传导膜;含有该固体电解质、隔板和/或电极的电化学电池;以及在混合物中存在的固体物质在电化学电池内改进周期稳定性的应用。
电化学电池、尤其可充电的电池一般可从例如“乌氏工业化学大全(Ullmann’s Encyclopedia of Industrial Chemistry)”,第五版,A3卷,VCH Verlagsgesellchaft mbH,Weinheim,1985,343-397页中获知。
在这些电池当中,锂电池和锂离子电池是尤为重要的,尤其作为二次电池,归因于它们较高的比能贮存密度。
正如以上“乌氏(Ullmann)”中所描述的,此类电池的阳极包括含有锰、钴、钒或镍的锂化混合氧化物,如按照化学计量最简单的情况,被描述为LiMn2O4,LiCoO2,LiV2O5或LiNiO2。
这些混合氧化物与能够将锂离子引入其晶格中的化合物如石墨进行可逆反应,从晶体的晶格中除去少量锂离子,在这一过程中,金属离子如锰、钴或镍离子被氧化。这一反应能够用于电化学电池中的电流贮备,这是借助于电解质来分离接受锂离子的化合物即阳极材料,和含锂混合氧化物即阴极材料,由此使锂离子从混合氧化物迁移到阳极材料中(充电过程)。
在这种情况下,通常使用粘结剂将适合于锂离子的可逆贮存的化合物固定到放电电极上。
当电池充电时,电子通过外部电压源和锂阳离子通过电解质到达阳极材料。当使用电池时,锂阳离子通过电解质而同时电子通过负载电阻从阳极材料到达阴极材料。
为了避免电化学电池内的短路,在两电极之间有一隔层,它是电绝缘的,但是锂阳离子的导体。该层可以是固体电解质或常规的隔板。
固体电解质和隔板已知是由载体材料组成,在载体材料中引入以提高锂离子传导性的含锂阳离子的可离解化合物和常规的其它添加剂如溶剂。
迄今公知的载体材料有US-A 5,296,318,US-A 5,429,891公开的内偏二氟乙烯和六氟丙烯的共聚物,这类高电阻(共)聚合物的应用具有一系列缺点。
此类聚合物不仅昂贵,而且很难溶解。此外,它们提高电池的电阻,这是归因于它们较低的锂阳离子传导率,这样在制备绝缘层时,必须加入主要由含锂阳离子的化合物如LiPF6、LiAsF6或LiSbF6和有机溶剂如碳酸亚乙酯或碳酸亚丙酯组成的电解质(US-A5,296,318,US-A5,429,891)。而且,此类聚合物仅在添加大量的增塑剂例如邻苯二甲酸二正丁酯和煅制硅酸是可以加工的,为的是,一方面,确保足够的成膜性和电解质层的附着力,以及与电解质层的可粘结性,另一方面,确保对锂阳离子有足够的传导率和渗透性。随后必须从由阳极、固体电解质层或隔离层和阴极层组成的层复合物中定量除去增塑剂,这要在电池投运之前以工业规模上是极其困难和昂贵的提取步骤进行。
此外,已知的是基于聚烯化氧的固体电解质,例如被描述在EP-A559317,EP-A576686,EP-A537930,EP-A585072和US5279910。其中所述的聚醚在其端基或官能团上被改性,例如借助于(甲基)丙烯酰基,并在使用之前由引入能量(热和光)使之交联。另外,它们一般包括导电性盐,例如LiPF6,以改进它们的导电性。其中没有描述在改进固体电解质的机械、热和电强度方面的固体物质的使用。显然,其中描述的体系,虽然已经交联,并不总是显示出就机械强度、所得膜材的孔隙率和抗短路性而言的令人满意的特性,
因此,本发明的目的是弥补这些缺点和提供尤其适合于制备固体电解质和隔板的混合物,但它们还可以用于制备电化学电池中的电极和用于这里所述的其它应用中。
由于存在下面将要描述的固体Ⅲ,与早已公知的体系相比本发明的混合物的使用将得到显示出改进的抗短路性能、高的耐压性能,尤其在高于120℃的高温下和较低孔隙率的固体电解质、隔板或电极,进一步能够持续抑制锂树枝晶的形成。还有,固体的存在将在电化学电池中获得改进的周期稳定性和高的电流可负荷性。当使用所优选使用的碱性固体时,在电化学电池的运行中所形成的酸会被中和或捕获。
因此,在一个实施方案中,本发明涉及一种混合物Ⅰa,该混合物包含由以下组分组成的组合物Ⅱa:
a)1-95%(重量)的固体物质Ⅲ,优选碱性固体物质Ⅲ,具有主要粒度为5nm-20μm,和
b)5-99%(重量)的通过聚合b1)和b2)所获得的聚合物Ⅳ:
b1)按物质Ⅵ计,5-100%(重量)的以下组分的缩合产物Ⅴ
α)至少一种能够与羧酸或磺酸或其衍生物或其两种或多种的组合物反应的化合物Ⅵ,和
β)对于每摩尔化合物Ⅵ而言至少1摩尔的具有至少一个可自由基聚合的官能团的羧酸或磺酸Ⅶ,或其衍生物或其两种或多种的混合物
和
b2)按物质Ⅳ计,0-95%(重量)的具有平均分子量(均数)为至少5000和在主链或侧链上具有聚醚链段的其它化合物Ⅷ,
其中混合物Ⅰa中组合物Ⅱa的重量比例是1-100%(重量)。
优选地,以上混合物Ⅰa是包括由以下组分组成的组合物Ⅱa的混合物:
a)1-95%(重量)的固体物质Ⅲ,优选为碱性固体物质Ⅲ,具有主要粒度为5nm-20μm,和
b)5-99%(重量)的通过聚合b1)和b2)所获得的聚合物Ⅳ:
b1)按物质Ⅳ计,5-100%(重量)的以下组分的缩合产物Ⅴ
α)主链含有碳原子和氧原子的多元醇Ⅵ,和
β)对于每摩尔多元醇Ⅵ而言至少1摩尔的α,β-不饱和羧酸Ⅶ,
和
b2)按物质Ⅳ计,0-95%(重量)的具有平均分子量(均数)为至少5000和在主链或侧链上具有聚醚链段的其它化合物Ⅷ,
其中混合物Ⅰa中组合物Ⅱa的重量比例是1-100%(重量)。
在另一个实施方案中,本发明涉及包括组合物Ⅱb的混合物Ⅰb,该组合物Ⅱb由以下组分组成:
a)1-95%(重量)的固体物质Ⅲ,优选为碱性固体物质Ⅲ,具有主要粒度为5nm-20μm,和
b)5-99%(重量)的通过聚合b1)和b2)所获得的聚合物Ⅸ:
b1)按聚合物Ⅸ计,5-75%(重量)的能够进行自由基聚合的、且与羧酸或磺酸Ⅶ或其衍生物不同的不饱和化合物Ⅹ或其两种或多种的组合物,
和
b2)按聚合物Ⅸ计,25-95%(重量)的具有平均分子量(均数)为至少5000和在主链或侧链上具有聚醚链段的其它化合物Ⅷ,
其中混合物Ⅰa中组合物Ⅱa的重量比例是1-100%(重量)。
合适的固体物质Ⅲ主要是无机固体物质,优选为无机碱性固体物质,它选自元素周期表Ⅰ、Ⅱ、Ⅲ或Ⅳ主族或Ⅳ副族的元素的氧化物,混合氧化物,硅酸盐,硫酸盐,碳酸盐,磷酸盐,氮化物,氨化物,亚胺化物和碳化物;聚合物,它选自聚乙烯、聚丙烯、聚苯乙烯、聚四氟乙烯、聚偏氟乙烯,聚酰胺,聚酰亚胺;含此类聚合物的固体分散体;和上述两种或多种的组合物。
作为例子,尤其可列举:
氧化物类,例如硅石、氧化铝、氧化镁或氧化钛,和混合氧化物类例如元素硅、钙、铝、镁和钛的混合氧化物;硅酸盐类,例如梯形硅酸盐类,具有链结构的硅酸盐类,层状硅酸盐,和网硅酸盐类;硫酸盐类,如碱金属和碱土金属硫酸盐;碳酸盐类,例如,碱金属和碱土金属碳酸盐例如钙、镁或钡碳酸盐或锂、钾或钠碳酸盐;磷酸盐类例如磷灰石;氮化物;氨化物;亚胺化物;碳化物;和聚合物类,例如聚乙烯、聚丙烯、聚苯乙烯、聚四氟乙烯;聚偏氟乙烯;聚酰胺;聚酰亚胺;或其它热塑性塑料、热固性塑料或微凝胶,固体物质分散体,尤其包括上述聚合物的那些,以及此类固体物质中两种或多种的混合物。
特别合适的是碱性固体物质,它被理解为这样一些物质:它们与本身pH最大为7的液体含水稀释剂的混合物具有比稀释剂的pH值要高的pH值。
理想的是,固体物质在用作电解质的液体中极难溶解,和在电池介质中表现电化学惰性。
特别合适的固体物质是具有主要粒度为5μm-20μm、优选0.01-10μm和尤其0.1-5μm的那些固体物质,所给出的粒度是由电子显微镜测得的。固体物质的熔点优选高于电化学电池的常规操作温度,即高于120℃,尤其高于150℃的熔点已被证明是特别有利的。
固体物质就它们的形状来说具有对称性,即它们显示出的尺寸比高度∶宽度∶长度(外观比)是大约1,并可以是球形、粒状、近圆形,但也可以显示出任何多面体的形状,例如立方形、四面体、六面体、八面体或双棱锥形,或可以是扭曲或不对称形状,即可以显示出尺寸比高度∶宽度∶长度(外观比)是不等于1,并可以是例如针形、不对称四面体、不对称双棱锥形、不对称六面体或八面体、小片形、盘形或纤维体的形状。对于固体为不对称颗粒时,上述主要粒度的上限与最短的轴有关。
作为能够与羧酸或磺酸或两者衍生物或其两种或多种的混合物反应的化合物Ⅵ,可使用所有满足这一标准的化合物。
优选地,化合物Ⅵ选自:
主链仅含碳原子的一元醇或多元醇;主链除具有至少两个碳原子还具有至少一个选自氧、磷和氮的原子的一元醇或多元醇;含硅化合物;包括至少一个伯胺基的胺类;包括至少一个仲胺基的胺类;氨基醇;一元或多元硫醇;具有至少一个硫醇和至少一个羟基的化合物;和上述化合物中两种或多种的组合物。
这些化合物当中,具有两个或多个能够与羧酸或磺酸反应的官能团的化合物Ⅵ是优选的。
当使用包括氨基作为官能团的化合物Ⅵ时,优选的是使用带仲胺基的那些,使得在缩合/交联之后没有或仅少量的游离NH基存在于混合物Ⅰa中。
作为优选的化合物,可提及以下这些:
主链仅含碳原子的一元醇或多元醇,它含有1-20个、优选2-20个和尤其2-10个醇式OH基,尤其是二、三或四元醇类,优选具有2-20个碳原子的那些醇类,如乙二醇、丙烷-1,2-或-1,3-二醇、丁烷-1,2-或-1,3-二醇、丁烯-1,4-或丁炔-1,4-二醇、己烷-1,6-二醇、新戊基二醇、十二烷-1,2-二醇、甘油、三羟甲基丙烷、季戊四醇或糖醇、氢醌,清漆型双酚A,其中从以上定义可以推断,可使用一元醇,如甲醇、乙醇、丙醇、正丁醇、仲丁醇或叔丁醇等;此外还可使用多羟基烯烃,优选具有两个端羟基的那些烯烃,例如α,ω-二羟基丁二烯;聚酯多元醇,例如从“乌氏技术化学大全”,第四版,19卷,62-65页中已知的那些,例如通过二元醇与多元、优选二元多羧酸反应获得;
除具有至少两个碳原子还具有至少一个氧原子的一元醇或多元醇,优选聚醚醇,例如烯化氧的聚合产物,例如异丁烯环氧化物,环氧丙烷,环氧乙烷,1,2-环氧基丁烷,1,2-环氧基戊烷,1,2-环氧基己烷,四氢呋喃,苯乙烯氧化物,还包括在端基改性的聚醚醇,如被NH2-端基改性的聚醚醇;具有分子量(均数)100-5000,更优选200-1000和尤其300-800的那些醇类;此类化合物是已知的并且例如能够以商标Pluriol或Pluronic(BASF AG)购得;
如以上所定义的醇类,其中部分或所有的碳原子被硅取代,尤其是聚硅氧烷或烯化氧和硅氧烷的共聚物或聚醚醇和聚硅氧烷的混合物,例如如EP-B581296和EP-A525728中所述的都是可以使用的,这些醇的分子量如以上所规定;
如以上所定义的醇类,尤其聚醚醇,其中部分或全部的氧原子被硫原子取代,也具有以上所列出的分子量;
除在主链上包括至少两个碳原子外还包括至少一个磷或至少一个氮原子的一元醇或多元醇,如二乙醇胺和三乙醇胺;
从通式HO-(CH2)z-COOH的化合物得到的内酯,其中z是1-20中的数字,如ε-己内酯、β-丙内酯、γ-丁内酯或甲基-ε-己内酯;
含硅化合物,如二或三氯硅烷、苯基三氯硅烷、二苯基二氯硅烷、二甲基乙烯氯硅烷;
硅烷醇类,如三甲基硅烷醇;
包括至少一个伯和/或仲胺基的胺类,如丁基胺、2-乙基己基胺、乙二胺、六亚甲基二胺、二亚乙基三胺、四亚乙基五胺、五亚乙基六胺、苯胺或苯二胺;
聚醚胺,如4,7-二氧基癸烷-1,10-二胺或4,11-二氧基十四烷-1,14-二胺;
一元或多元硫醇,例如脂族硫醇如甲烷硫醇、乙烷硫醇、环己烷硫醇、十二烷硫醇;芳族硫醇如苯硫酚、4-氯苯硫酚、2-巯基苯胺;
包含至少一个硫醇和至少一个羟基的化合物,如4-羟基苯硫酚,和以上所定义多元醇的一元硫醇衍生物;
氨基醇类,如2-氨基乙醇、N-甲基-2-氨基乙醇、N-乙基-2-氨基乙醇、N-丁基-2-氨基乙醇、2-氨基-1-丙醇、2-氨基-1-苯酚乙醇、具有两个以上脂族基连接的羟基的单或多氨基醇,如三(羟甲基)甲基胺、胍或N,N’-双(2-羟乙基)乙二胺。
还可以使用以上所定义化合物Ⅵ中的两种或多种的混合物。
根据本发明,以上所定义的化合物Ⅵ与具有至少一个自由基可聚合的官能团的羧酸或磺酸Ⅶ,或其衍生物或其两种或多种的混合物进行缩合反应,据此,化合物Ⅵ中至少一个,优选所有能够缩合的游离基与化合物Ⅶ缩合。
在本发明中,一般具有至少一个可自由基聚合的官能团的所有羧酸和磺酸,或其衍生物能够用作羧酸或磺酸Ⅶ。术语“衍生物”包括从在酸官能团上改性的羧酸或磺酸得到的化合物,如酯、酰氯或酸酐,和从羧酸或磺酸得到的化合物,它们在羧酸或磺酸的碳骨架上被改性,如卤代羧酸或磺酸。
作为化合物Ⅶ,尤其可提及以下这些:
α,β-不饱和羧酸或β,γ-不饱和羧酸。
特别合适的α,β-不饱和羧酸是具有下式的那些:其中R1、R2和R3是氢或C1-C4烷基,其中丙烯酸和甲基丙烯酸是优选的;其它合适的化合物是肉桂酸、马来酸、富马酸、衣康酸或对-乙烯基苯甲酸,和其衍生物,如酸酐例如马来酸酐或衣康酸酐;
卤化物,尤其氯化物,如丙烯酰或甲基丙烯酰氯;
酯,例如在烷基上具有至多20个碳原子的(甲基)丙烯酸(环)烷基酯,如甲基-、乙基-、丙基-、丁基-、己基-、2-乙基己基-、硬脂基-、月桂基-、环己基-、苄基-、三氟甲基-、六氟丙基-、四氟丙基(甲基)丙烯酸酯,聚丙二醇单(甲基)丙烯酸酯,聚乙二醇单(甲基)丙烯酸酯,多元醇的聚(甲基)丙烯酸酯,如二(甲基)丙烯酸甘油酯,二(甲基)丙烯酸(三羟甲基丙烷)酯,二(甲基)丙烯酸季戊四醇酯或三(甲基)丙烯酸季戊四醇酯,双(单-(2-丙烯酰氧基)乙基)碳酸二乙二醇酯,具有自由基可聚合基团的醇的聚(甲基)丙烯酸酯,如(甲基)丙烯酸和乙烯和/或烯丙基醇的酯;
其它脂族或芳族羧酸的乙烯基酯,如乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、己酸乙烯酯、辛酸乙烯酯、癸酸乙烯酯、硬脂酸乙烯基酯、棕榈酸乙烯基酯、巴豆酸乙烯基酯、己二酸二乙烯基酯、癸二酸二乙烯基酯、己酸2-乙烯基-2-乙基酯、三氟乙酸乙烯基酯;
其它脂族或芳族羧酸的烯丙基酯,如乙酸烯丙基酯、丙酸烯丙基酯、丁酸烯丙基酯、己酸烯丙基酯、辛酸烯丙基酯、硅酸烯丙基酯、硬脂酸烯丙基酯、棕榈酸烯丙基酯、巴豆酸烯丙基酯、水杨酸烯丙基酯、乳酸烯丙基酯、草酸烯二烯丙基酯、丙二酸二烯丙基酯、琥珀酸二烯丙基酯、戊二酸二烯丙基酯、己二酸二烯丙基酯、庚二酸二烯丙基酯、肉桂三羧酸二烯丙基酯、三氟乙酸烯丙基酯、全氟丁酸烯丙基酯、全氟辛酸烯丙基酯;
β,γ-不饱和羧酸或其衍生物,如乙烯基乙酸、2-甲基乙烯基乙酸、3-丁烯酸异丁基酯、3-丁烯酸烯丙基酯、2-羟基-3-丁烯酸烯丙基酯、双烯酮。
磺酸,如乙烯基磺酸、烯丙基-和甲基烯丙基磺酸,和其酯和酰卤,乙烯苯磺酸盐,4-乙烯基苯砜酰胺。
还可以上述羧酸和/或磺酸的两种或多种的组合物。
作为能够进行自由基聚合以制备聚合物Ⅸ的化合物Ⅹ,可提及下列这些:
烯属烃类,如乙烯、丙烯、丁烯、异丁烯、己烯、或较高同系物,和乙烯基环己烷;
(甲基)丙烯腈;
含卤素的烯烃化合物,如偏二氟乙烯、偏二氯乙烯、氟乙烯、氯乙烯、六氟丙烯、三氟丙烯、1,2-二氯乙烯、1,2-二氟乙烯和四氟乙烯;
乙烯醇、乙酸乙烯酯、N-乙烯基吡咯烷酮、N-乙烯基咪唑、乙烯甲酰胺;
氯化氮化磷类,如二氯化氮化磷、六氯(三磷腈)、以及其被烷氧基-、苯氧基-、氨基-和氟烷氧基残基部分地或完全取代的衍生物,即可聚合成聚(磷腈)的化合物;
芳族烯烃化合物,如苯乙烯、α-甲基苯乙烯;
乙烯基醚,如甲基-、乙基-、苄基-、异丙基-、丁基-、异丁基-、己基-、辛基-、癸基-、十二烷基-、2-乙基己基-、环己基-、苄基-、三氟甲基-、六氟丙基-、四氟丙基乙烯基醚。
还可以使用上述化合物Ⅹ的混合物,取决于制备方法而制得的具有单体统计分布的共聚物或得到嵌段共聚物。
这些化合物Ⅹ以及缩合产物Ⅴ是通过本技术领域中熟练人员已知的普通方法,优选自由基聚合反应,进行聚合。对于所获得的分子量,参见后面对有关化合物Ⅷ的讨论。
作为特别合适的化合物Ⅷ是具有平均分子量(均数)为至少5,000,优选5,000-20,000,000,尤其100,000-6,000,000的化合物,它能够将锂阳离子加以溶剂化并用作粘结剂。合适的化合物Ⅷ例如是聚醚和共聚物,按化合物Ⅷ的总重量计,它包括至少30%(重量)的以下结构单元:其中R1、R2、R3和R4表示芳基,烷基,优选甲基,或氢,该残基可以相同或不同并可含有杂原子,如氧、氮、硫或硅。
此类化合物例如描述在M.B.Armand等人,“固体中的离子快转移”(FastIon Transport in Solids),E1sevier,New York,1979,S.131-136或在FR-A-7832976。
化合物Ⅷ还可由这些化合物中两种或多种的混合物组成。
以上所定义的聚合物Ⅳ和聚合物Ⅸ分别也能够以海绵状存在,其中固体物质Ⅲ被分布在其中。
根据本发明,组合物Ⅱa应该由1-95%(重量),优选25-90%(重量)和,尤其30-70%(重量)的固体物质Ⅲ和5-99%(重量)、优选10-75%(重量)和尤其30-70%(重量)的聚合物Ⅳ组成,其中聚合物Ⅳ的化合物Ⅷ理想地具有平均分子量(均数)为5,000-100,000,000,优选50,000-8,000,000。聚合物Ⅳ可通过按聚合物Ⅳ计的5-100%(重量)、优选30-70%(重量)的化合物Ⅴ和按聚合物Ⅳ计的0-95%(重量)、尤其30-70%(重量)的化合物Ⅷ反应而获得。
根据本发明,组合物Ⅱb应该由1-95%(重量),优选25-90%(重量)和尤其30-70%(重量)的固体物质Ⅲ和5-99%(重量)、优选10-75%(重量)和尤其30-70%(重量)的聚合物Ⅸ组成,其中聚合物Ⅸ的化合物Ⅷ应该优选具有平均分子量(均数)为5,000-100,000,000,优选50,000-8,000,000。聚合物Ⅸ可通过按聚合物Ⅸ计,5-75%(重量)、优选30-70%(重量)的化合物Ⅹ和按聚合物Ⅸ计,25-95%(重量)、尤其30-70%(重量)的化合物Ⅷ反应而获得。
在下文中,混合物Ⅰa和Ⅰb以及根据本发明的组合物Ⅱa和Ⅱb在下文中一起讨论并表示为“根据本发明的混合物”和“根据本发明的组合物”。
为了获得本发明的混合物,该混合物欲含按本发明的混合物计为1-100%(重量)、优选35-100%(重量)和尤其30-70%(重量)的组合物,则有可能制备由固体物质Ⅲ,缩合产物Ⅴ,还可以有化合物Ⅷ或固体物质Ⅱ、化合物Ⅹ和化合物Ⅷ的组合物,和常规添加剂如增塑剂,优选含有聚氧化乙烯或聚氧化丙烯类的增塑剂组成的组合物。
作为增塑剂,可使用以下化合物:
非质子传递溶剂,优选将Li离子加以溶剂化的那些,例如碳酸二甲酯,碳酸二乙酯,碳酸二丙酯,碳酸二异丙酯,碳酸二丁酯,碳酸亚乙基酯,碳酸亚丙基酯;低聚烯化氧,如二丁基醚,二叔丁基醚,二苯基醚,二己基醚,二庚基醚,二辛基醚,二壬基醚,二癸基醚,双十二烷基醚,乙二醇二甲醚,乙二醇二乙醚,1-叔丁氧基-2-甲氧基乙烷,1-叔丁氧基-2-乙氧基乙烷,1,2-二甲氧基丙烷,2-甲氧基乙基醚,2-乙氧基乙基醚,二乙二醇二丁基醚,二亚甲基二醇-叔丁基甲基醚,三乙二醇二甲基醚,四乙二醇二甲基醚,γ-丁内酯,二甲基甲酰胺;具有通式CnH2n+2的烃类,其中7<n<50;有机磷化合物,尤其磷酸盐和膦酸盐如磷酸三甲基酯,磷酸三乙基酯,磷酸三丙基酯,磷酸三丁基酯,磷酸三异丁基酯,磷酸三戊基酯,磷酸三己基酯,磷酸三辛基酯,磷酸三(2-乙基己基)酯,磷酸三癸基酯,磷酸二乙基正丁基酯,磷酸三(丁氧基乙基)酯,磷酸三(2-甲氧基乙基)酯,磷酸三(四氢呋喃基)酯,磷酸三(1H,1H,5H-八氟戊基)酯,磷酸三(1H,1H-三氟乙基)酯,磷酸三(2-(二乙基氨基)乙基)酯,膦酸二乙基乙基酯,膦酸二丙基丙基酯,膦酸二丁基丁基酯,膦酸二己基己基酯,膦酸二辛基辛基酯,膦酸乙酸乙基二甲基酯,膦酸乙酸甲基二乙基酯,膦酸乙酸三乙基酯,膦酸二甲基(2-氧代丙基)酯,膦酸二乙基(2-氧代丙基)酯,膦酸二丙基(2-氧代丙基)酯,二乙氧基氧膦基甲酸乙酯,三甲基膦酸乙酸三甲基酯,膦酸乙酸三乙基酯,膦酸乙酸三丙基酯,膦酸乙酸三丁基酯;有机硫组分如硫酸盐,磺酸盐,亚砜,砜,和亚硫酸酯如亚硫酸二甲酯,亚硫酸二乙基酯,亚硫酸二醇酯,二甲基砜,二乙基砜,二乙基丙基砜,二丁基砜,四亚甲基砜,甲基环丁砜,二甲基亚砜,二乙基亚砜,二丙基亚砜,二丁基亚砜,四亚甲基亚砜,乙基甲烷磺酸盐,1,4-丁二醇双(甲烷磺酸盐),硫酸二乙基酯,硫酸二丙基酯,硫酸二丁基酯,硫酸二己基酯,硫酸二辛基酯;SO2ClF;腈类,如丙烯腈;
分散剂,特别是具有表面活性剂结构的那些;
以及它们的组合物。
本发明的混合物可溶于和分散于无机液体稀释剂中,但优选溶于和分散于有机液体稀释剂中,由此本发明的混合物应具有粘度优选为100-50,000mPas,然后按照已知的方法借助于喷涂、倾注、浸泡、旋转涂敷、辊涂或印刷如通过凸印、凹印、平版印刷或丝网印刷将这一溶液或分散液涂敷到载体材料上。随后的处理由常规方法进行,例如除去稀释剂和固化粘结剂。
合适的有机稀释剂是脂族醚,尤其四氢呋喃和二噁烷,烃类,尤其烃混合物如石油精,甲苯和二甲苯,脂族酯类,尤其乙酸乙酯和乙酸丁酯,和酮类,尤其丙酮,乙基甲基酮和环己酮。能够使用此类稀释剂的混合物。
合适的载体材料是常常用于电极的那些材料,优选诸如铝和铜的金属。还有可能是临时的中间载体,如膜材,尤其聚酯膜如聚对苯二甲酸乙二醇酯膜。此类膜上最好带有脱膜层,优选为聚硅氧烷层。
固体电解质和隔板的制备也能够通过热塑性塑料加工方法来进行,例如通过注塑,倾注,压塑,捏合或挤出,还可以有本发明所述混合物的随后压延步骤。
在本发明的混合物成膜后,可除去挥发性组分如溶剂或增塑剂。
本发明的混合物能够按已知的方式进行交联,例如通过用离子或电离辐射,电子束,优选在20-2000kV的加速电压和5-50Mrad(百万拉德)的辐射剂量下,或用UV或可见光,在这种情况下,与常规情况一样,最好将一种引发剂如苯偶酰二甲基缩酮或1,3,5-三甲基-苯甲酰基三苯基膦氧化物以按聚合物组合物Ⅳ或聚合物Ⅸ计最大以1%(重量)的量添加,以及交联反应最好在0.5-15分钟内在惰性气体如氮气或氩气下,借助于热自由聚合反应,优选在高于60℃的温度下完成,最好按聚合物组合物Ⅳ或聚合物Ⅸ计最大以5%(重量)、优选0.05-1%(重量)的量添加引发剂如偶氮二异丁腈,借助于电化学诱发的聚合反应,或借助于离子聚合反应,例如通过酸催化的阳离子聚合反应进行,在这种情况下首选酸作催化剂,优选是路易斯酸如BF3,或尤其LiBF4或LiPF6。在这种情况下,含有锂离子的催化剂如LiBF4或LiPF6作为导电性盐保留在固体电解质或隔板中是有利的。
如果将本发明的混合物用作电化学电池中的固体电解质或隔板,则引入可离解的含锂阳离子化合物即所谓导电性盐,以及还可引入其它添加剂如尤其是有机溶剂即所谓电解质。
这些物质可以在混合物层的制备过程中被部分地或全部地混合,或在制备之后引入层中。
作为导电性盐,可使用通常已知的导电性盐类,例如描述在EP-A96629中那些。特别合适的是诸如LiPF6,LiAsF6,LiSbF6,LiClO4,LiN(CF3SO2)2,LiBF4或LiCF3O3和其混合物。这些导电性盐的用量按本发明组合物计为0.1-20%(重量),优选1-10%(重量)。
作为有机电解质,可以使用以上关于“增塑剂”所讨论的化合物,优选为常用的有机电解质,可以使用酯类如碳酸亚乙基酯,碳酸亚丙基酯,碳酸二甲基酯和碳酸二乙基酯或其混合物。
适合于电化学电池的本发明的固体电解质、隔板和/或电极最好具有厚度5-500微米,优选10-500微米,更优选10-200微米和尤其20-100微米。
当用本发明混合物作阴极或用于制备阴极时,可以引入通常用于阴极的化合物(阴极化合物)的导电性电化学活性化合物,优选锂化合物。尤其可列举:
LiCoO2,LiNiO2,LixMnO2(0<x≤1),LixMn2O4(0<x≤2),LixMoO2(0<x≤2),LixMnO3(0<x≤1),LixMnO2(0<x≤2),LixMn2O4(0<x≤2),LixV2O4(0<x≤2.5),LixV2O3(0<x≤3.5),LixVO2(0<x≤1),LixWO2(0<x≤1),LixWO3(0<x≤1),LixTiO2(0<X≤1),LixTi2O4(0<x≤2),LixRuO2(0<x≤1),LixFe2O3(0<x≤2),LixFe3O4(0<x≤2),LixCr2O3(0<x≤3),LixCr3O4(0<x≤3.8),LixV3S5(0<x≤1.8),LixTa2S2(0<x≤1),LixFeS(0<x≤1),LixFeS2(0<x≤1),LixNbS2(0<x≤2.4),LixMoS2(0<x≤3),LixTiS2(0<x≤2),LixZrS2(0<x≤2),LixNbSe2(0<x≤3),LixVSe2(0<x≤1),LixNiPS2(0<x≤1.5),LixFePS2(0<x≤1.5)。
当用作阳极时,作为阳极材料,可引入现有技术中已知的导电性电化学活性化合物(阳极化合物),尤其列举以下化合物:
锂,含锂的合金,微米级炭黑,天然和合成石墨,合成的石墨化碳灰,和碳纤维,氧化物类如氧化钛、氧化锌、氧化锡、氧化钼、氧化钨,碳酸盐类如碳酸钼和碳酸锌。
当用作制备阳极或用作阳极时,向本发明的混合物中引入按混合物的总重量计的至多20%(重量)的导电性炭黑和还可有上述的常用添加剂。当用于制备阴极或用作阴极时,混合物含有按混合物的总重量计的0.1-20%(重量)的导电性炭黑。
本发明的混合物在电化学电池中可单独作为固体电解质和/或隔板和/或电极使用,或与另外的固体电解质、隔板和/或电极形成组合物使用。
此外,本发明涉及一种复合体,它以膜的形式,优选以总厚度15-1,500微米、尤其总厚度50-500微米的膜形式特别用于电化学电池中,该复合体包括至少一层含导电性的电化学活性化合物的第一层和至少一层含本发明的混合物而不含导电性的电化学活性化合物的第二层。
此外,本发明描述了制备该复合体的方法,包括以下步骤:
(Ⅰ)制备如以上所定义的至少一层第一层;
(Ⅱ)制备如以上所定义的至少一层第二层;
和
(Ⅲ)然后由常用涂敷方法将至少一层第一层和至少一层第二层组合。
优选地,在临时载体上制备至少一层第二层。根据本发明,可使用常用的临时载体,如由聚合物或优选涂层纸制备的分隔膜,如硅化聚酯膜。该第二层的制备也可在永久性载体如放电电极上制备,或没有任何载体。
以上所定义各层的组合和制备可通过涂敷膜或制备膜的无压方法来实现,如倾注或刮涂,以及通过加压方法,如挤出,层压,涂敷,压延或压制。还可以通过辐照、电化学或热方法实施所制备的复合体交联或固化。
当然,除以上所定义的第二层外,以上所定义的第一层也可包含本发明的混合物。
从以上可推断,还可提供具有隔离膜/隔板(第二层)/电极(第一层)组成的复合体。
此外,借助双侧涂敷法有可能获得具有阳极/隔板/阴极组成的复合体。
例如,可按以下进行:
首先,阳极材料,例如氧化锡,导电性炭黑,本发明的混合物,导电性盐和增塑剂例如碳酸亚丙基酯可以进行共混,所得到的混合物被倾注在放电电极上,随后由UV光辐照(组件1)。然后,阴极材料例如LiMn2O4被涂敷在已用导电性炭黑涂敷过的放电电极上,和将由本发明混合物、导电性盐和增塑剂的组合物倾注其上。同时,这一复合物随后由UV光辐照(组件2)。通过将上述两组件组合在一起,获得复合体,它们与自由选择的固体电解质和/或液体电解质组合在一起用作电化学电池。
无需使用载体或放电电极,如以上所述的阳极/隔板/阴极结构也能够制备,因为所获得的复合体由以上所定义的第一和第二层组成,本身所具有的机械稳定剂足以用于电化学电池中。
在两层组合之前或优选在组合两层之后,还可以在其与合适的放电电极例如金属膜接触之后,甚至可以在将复合物引入电池壳中后来对此类复合物填充电解质和导电性盐,并且,据此通过使用本发明的混合物获得具有特定微孔结构的各层,尤其归因于以上所定义固体物质在隔板和还可以在电极中的存在,使得在孔内电解质和导电性盐的吸附和孔内空气的排出成为可能。该填充可在0-约100℃范围内的温度下进行,取决于所使用的电解质。
本发明的电化学电池特别可用作汽车电池、仪器电池或扁平电池。
从以上可以推断,本发明还涉及本发明混合物或如以上所描述的复合体在固体电解质,隔板,电极,传感器,电致变色显示窗,显示器,电容器或离子导电膜的制备中的应用,以及,本发明涉及包含本发明的混合物或如以上所描述的复合物的固体电解质,隔板,电极,传感器,电致变色显示窗,显示器,电容器和离子导电膜。
再者,本发明涉及电化学电池,它包含如以上所定义的固体电解质、隔板或电极,或它们当中两种或多种的组合,以及本发明的电化学电池作为汽车电池、仪器电池或扁平电池的用途。
再者,本发明普遍涉及具有主粒度为5纳米-20微米的固体Ⅲ在固体电解质、隔板或电极中以提高电化学电池的周期稳定性的应用,因为在实现本发明的过程中,已经发现,此类固体物质的添加对电化学电池的这一特性具有极其有效的影响。
实施例
实施例1
使用高速搅拌器,将75g已用环氧基硅烷调节为疏水性的、具有平均粒度为3微米的硅灰石(Tremin800EST,购自QuarzwerkeFrechen公司),其水悬浮液具有pH值8.5,分散在300g甲苯中。向该混合物中添加12.5g的平均分子量(均数)为2,000,000的聚氧化乙烯(Polyox,购自联合碳化物公司)和12.5g的氧化丙烯-氧化乙烯嵌段共聚物的甲基丙烯酸二酯(PluriolPE600,购自BASF AG公司)和0.02g的UV光引发剂(LucirinBDK,购自BASF AG公司)。
使用缝宽300微米的刮刀,在60℃下将组合物涂敷到硅氧烷处理过的脱膜纸上,在5分钟内除去稀释剂,干燥的涂层取下后获得厚度约40微米的膜,在氩气气氛下通过在超锕系荧光灯(TL09,购自Philips公司)下方5cm的距离处曝光10分钟以进行光致交联。
挠性膜是具有优异挠曲强度。远低于1mm的弯曲半径仍能够承受且不会断裂。
甚至在室温下贮存2周以上后,膜仍然没有显示有球形聚氧化乙烯晶体,并在含有导电性盐的上述有机电解质中具有良好的抗溶胀性。
含有导电性盐的有机电解质通过自发向内扩散在几分钟内被充分吸收,溶胀低于50%(重量)。
溶胀膜具有良好的强度。
结果总结在表中。
实施例2
使用高速搅拌器,将60g具有平均粒度3微米的硅灰石,其水悬浮液具有pH值8.5,分散在200g四氢呋喃(THF)中。向该混合物中添加13.3g的平均分子量(均数)为2,000,000的聚氧化乙烯(Polyox,购自联合碳化物公司)、13.3g的氧化丙烯-氧化乙烯嵌段共聚物的甲基丙烯酸二酯(PluriolPE600,购自BASF AG公司)、13.3g的THF-可溶性偏二氟乙烯-六氟丙烯共聚物(Kynarflex2850,购自ELF-Atochem公司)和0.02g的UV光引发剂(LucirinBDK,购自BASF AG公司)。
使用缝宽500微米的刮刀,在60℃下将混合物涂敷到硅氧烷处理过的脱膜纸上,在5分钟内除去稀释剂,干燥的涂层取下后获得厚度约50微米的膜,在氩气气氛下通过在超锕系荧光灯(TL09,购自Philips公司)下方5cm的距离处曝光10分钟以进行光致交联。
挠性膜具有优异挠曲强度。远低于1mm的弯曲半径仍能够承受且不会断裂。
甚至在室温下贮存2周以上后,膜仍然没有显示有球形聚氧化乙烯晶体,并在含有导电性盐的上述有机电解质中具有良好的抗溶胀性。
含有导电性盐的有机电解质通过自发向内扩散在几分钟内被充分吸收,溶胀低于50%(重量)。
溶胀膜具有良好的强度。
结果总结在表中。
实施例3
使用高速搅拌器,将60g具有平均粒度3微米的石英粉(Silbond800EST,购自Quarzwerke Frechen公司),其水悬浮液具有pH值7.5,分散在250g四氢呋喃中。向该混合物中添加13.3g的平均分子量(均数)为3,000,000的聚氧化乙烯(Polyox,购自联合碳化物公司)、13.3g的氧化丙烯-氧化乙烯嵌段共聚物的甲基丙烯酸二酯(PluriolPE600,购自BASF AG公司),和13.3g的THF-可溶性偏二氟乙烯-六氟丙烯共聚物(Kynarflex2850,购自ELF-Atochem公司)。
使用缝宽500微米的刮刀,在60℃下将混合物涂敷到硅氧烷处理过的脱膜纸上,在5分钟内除去稀释剂,干燥的涂层取下后获得厚度约50微米的膜,在氮气气氛下通过在150kV的加速电压下以30Mrad的剂量用电子束辐照以进行交联。
挠性膜具有优异挠曲强度。远低于1mm的弯曲半径仍能够承受且不会断裂。
甚至在室温下贮存2周以上后,膜仍然没有显示有球形聚氧化乙烯晶体,并在含有导电性盐的上述有机电解质中具有良好的抗溶胀性。
含有导电性盐的有机电解质通过自发向内扩散在几分钟内被充分吸收,溶胀低于50%(重量)。
溶胀膜具有良好的强度。
结果总结在表中。
实施例4
使用高速搅拌器,将60g已用甲基丙烯酰基硅烷调节至疏水性的、具有平均粒度3微米的硅灰石,其水悬浮液具有pH值8.5,分散在200g四氢呋喃(THF)中。向该混合物中添加13.3g的平均分子量(均数)为2,000,000的聚氧化乙烯(Polyox,购自联合碳化物公司)、13.3g的氧化丙烯-氧化乙烯嵌段共聚物的甲基丙烯酸二酯(PluriolPE600,购自BASF AG公司)、13.3g的THF-可溶性偏二氟乙烯-六氟丙烯共聚物(Kynarflex2850,购自ELF-Atochem公司)和0.02g的偶氮二异丁腈。
使用缝宽500微米的刮刀,在60℃下将混合物涂敷到硅氧烷处理过的脱膜纸上,在5分钟内除去稀释剂,干燥的涂层取下后获得厚度约50微米的膜,在氮气气氛下通过在超锕系荧光灯(TL09,购自Philips公司)下方5cm的距离处曝光10分钟以进行光致交联。
挠性膜具有优异挠曲强度。远低于1mm的弯曲半径仍能够承受且不会断裂。
甚至在室温下贮存2周以上后,膜仍然没有显示有球形聚氧化乙烯晶体,并在含有导电性盐的上述有机电解质中具有良好的抗溶胀性。
含有导电性盐的有机电解质通过自发向内扩散在几分钟内被充分吸收,溶胀低于50%(重量)。
溶胀膜具有良好的强度。
结果总结在表中。
实施例5
实施例5主要与实施例1相同,然而,区别在于:
一代替Tremin600EST,使用Tremin939-600MST,即一种已用甲基丙烯酰基硅烷调节至疏水性的、具有平均粒度为3.5微米的呈现针形的硅灰石,
-代替PluriolPE600,使用PluriolE600,即一种氧化乙烯聚合物,用量同实施例1;和
-用于将所获得组合物涂敷在硅氧烷处理过的脱膜纸上的刮刀具有缝宽200微米。
根据实施例1加以处理后的膜的结果示于表中。
对比实施例1
将12.5g的平均分子量(均数)为2,000,000的聚氧化乙烯(Polyox,购自联合碳化物公司),12.5g的氧化丙烯-氧化乙烯嵌段共聚物的甲基丙烯酸二酯(PluriolPE600,购自BASF AG公司)和0.02g的光引发剂(LucirinBDK,购自BASF AG公司)溶于200g四氢呋喃中。
使用缝宽750微米的刮刀,在60℃下将混合物涂敷到硅氧烷处理过的脱膜纸上,在5分钟内除去稀释剂,干燥的涂层取下后获得厚度约40微米的膜,在氩气气氛下通过在超锕系荧光灯(TL09,购自Philips公司)下方5cm的距离处曝光10分钟以进行光致交联。
挠性膜具有优异挠曲强度。远低于1mm的弯曲半径仍能够承受且不会断裂。甚至在室温下贮存2周以上后,膜仍然没有显示有球形聚氧化乙烯晶体,并在含有导电性盐的上述有机电解质中具有良好的抗溶胀性。
含有导电性盐的有机电解质通过自发向内扩散在几分钟内被充分吸收,溶胀低于150%(重量),膜尺寸和厚度有显著的变化。
强度大大低于实施例1-3。
在锂离子电池中,由于有过大的自放电速率或微短路,在所有情况下该膜导致电池破坏。
结果总结在表中。
对比实施例2
使用高速搅拌器,将75g已用环氧基硅烷调节至疏水性的、具有平均粒度3微米的硅灰石(Tremin800EST,购自Quarzwerke Frechen公司),其水悬浮液具有pH值8.5,分散在300g甲苯中。向该混合物中添加12.5g的平均分子量(均数)为2,000,000的聚氧化乙烯(Polyox,购自联合碳化物公司)、12.5g的氧化丙烯-氧化乙烯嵌段共聚物的甲基丙烯酸二酯(PluriolPE600,购自BASF AG公司),和0.02g光引发剂(LucirinBDK,购自BASF AG公司)。
使用缝宽300微米的刮刀,在60℃下将混合物涂敷到硅氧烷处理过的脱膜纸上,在5分钟内除去稀释剂,干燥的涂层取下后获得厚度约40微米的膜。
挠性膜是具有优异挠曲强度。远低于1mm的弯曲半径仍能够承受且不会断裂。
甚至在室温下贮存2周以上后,膜仍然显示有小的圆球形聚氧化乙烯晶体,并在含有导电性盐的上述有机电解质中不具有良好的抗溶胀性。在几分钟的溶胀时间过后,形成裂纹或膜变粘性,结果是溶胀后的膜无法再进行处理。
结果总结在表中。
对比实施例3
根据US-A5,429,891的实施例1(F),向30g的偏二氟乙烯-六氟丙烯共聚物(Kynarflex2822,购自ELF-Atochem公司)、20g的硅烷化热解硅酸(Aerosil R974,购自Degussa公司),其水悬浮液具有pH值7,50g的邻苯二甲酸二丁基酯(Palatinol C,购自BASF AG公司)和200g的丙酮的混合物中添加按邻苯二甲酸二丁基酯计为5%(重量)的三甲基丙烯酸三羟甲基丙烷酯。
使用缝宽750微米的刮刀将这一组合物涂敷到玻璃板上,在空气流中干燥15分钟,和包埋在两片0.075mm厚的Mylar层之间。然后通过4.5MeV的电子以5Mrad的剂量进行辐照,使100微米的膜层被交联,每次辐照期为2.5Mrad的剂量。挠曲膜具有良好的挠曲强度。
在膜用于锂离子电池之前,通过萃取十分费力地除去增塑剂是必要的,否则由于电极受污染,仅仅获得不好的周期强度。为了除去增塑剂,膜需要在室温下进行5次萃取操作,每次持续10分钟,使用相当于膜重量50倍的乙醚。在除去增塑剂之后,膜是不稳定的和在弯曲时易发生断裂。
不含增塑剂的膜在含有导电性盐的所述有机电解质中具有良好的抗溶胀性。
含有导电性盐的有机电解质通过自发向内扩散在几分钟内被充分吸收。
溶胀膜具有良好的强度。
结果总结在表中。
表
级别:1非常好2良好3令人满意4不好5差6太差无法进行试验
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 对比例1 | 对比例2 | 对比例3 | |
有增塑剂的强度 | - | - | - | - | - | - | - | 2 |
萃取 | - | - | - | - | - | - | - | 需要 |
没有增塑剂的强度 | 2 | 1 | 1 | 1 | 1 | 2 | 5 | 5 |
抗溶胀性 | 2 | 2 | 2 | 2 | 2 | 3 | 5 | 2 |
溶胀后的强度 | 2 | 2 | 2 | 2 | 2 | 4 | 6 | 2 |
导电性 | 2 | 2 | 2 | 2 | 1 | 2 | 4 | 2 |
抗短路性 | 1 | 1 | 1 | 1 | 1 | 4 | 6 | 1 |
电化学载荷容量 | 1 | 2 | 3 | 2 | 1 | 5 | 6 | 4 |
周期强度 | 1 | 1 | 1 | 1 | 1 | 5 | 6 | 2 |
Claims (12)
1.一种混合物Ⅰa,该混合物包含由以下组分组成的组合物Ⅱa:
a)1-95%(重量)的固体物质Ⅲ,优选为碱性固体物质Ⅲ,具有主要粒度为5nm-20μm,和
b)5-99%(重量)的通过聚合b1)和b2)所获得的聚合物Ⅳ:
b1)按物质Ⅳ计,5-100%(重量)的以下组分的缩合产物Ⅴ
α)至少一种能够与羧酸或磺酸或其衍生物或其两种或多种的组合物反应的化合物Ⅵ,和
β)对于每摩尔化合物Ⅵ而言至少1摩尔的具有至少一个可自由基聚合的官能团的羧酸或磺酸Ⅶ,或其衍生物或其两种或多种的组合物
和
b2)按物质Ⅳ计,0-95%(重量)的具有平均分子量(均数)为至少5000和在主链或侧链上具有聚醚链段的其它化合物Ⅷ,
其中混合物Ⅰa中组合物Ⅱa的重量比例是1-100%(重量)。
2.根据权利要求1的混合物,其中化合物Ⅵ选自:
主链仅含碳原子的一元醇或多元醇;主链除具有至少两个碳原子还具有至少一个选自氧、磷和氮的原子的一元醇或多元醇;含硅化合物;包括至少一个伯胺基的胺类;包括至少一个仲胺基的胺类;氨基醇;一元或多元硫醇;具有至少一个硫醇和至少一个羟基的化合物;和上述化合物中两种或多种的混合物。
3.根据权利要求1或2的混合物,其中羧酸或磺酸Ⅶ或其衍生物选自:α,β-不饱和羧酸或其衍生物,脂族或芳族羧酸的乙烯基酯,脂族或芳族羧酸的烯丙基酯,和上述化合物中两种或多种的组合物。
4.根据权利要求1-3中任何一项的混合物,其中组合物Ⅱa由以下组分组成:
a)1-95%(重量)的固体物质Ⅲ,优选为碱性固体物质Ⅲ,具有主要粒度为5nm-20μm,和
b)5-99%(重量)的通过聚合b1)和b2)所获得的聚合物Ⅳ:
b1)按物质Ⅳ计,5-100%(重量)的以下组分的缩合产物Ⅴ
α)主链含有碳原子和氧原子的多元醇Ⅳ,和
β)对于每摩尔多元醇Ⅵ而言至少1摩尔的α,β-不饱和羧酸Ⅶ
和
b2)按物质Ⅳ计,0-95%(重量)的具有平均分子量(均数)为至少5000和在主链或侧链上具有聚醚链段的其它化合物Ⅷ,
其中混合物Ⅰa中组合物Ⅱa的重量比例是1-100%(重量)。
5.一种混合物Ⅰb,该混合物包含由以下组分组成的组合物Ⅱb:
a)1-95%(重量)的固体物质Ⅲ,优选为碱性固体物质Ⅲ,具有主要粒度为5nm-20μm,和
b)5-99%(重量)的通过聚合b1)和b2)所获得的聚合物Ⅸ:
b1)按聚合物Ⅸ计,5-75%(重量)的能够进行自由基聚合的、且与羧酸或磺酸Ⅶ或其衍生物不同的化合物Ⅹ或化合物Ⅹ当中两种或多种的组合物,
和
b2)按聚合物Ⅸ计,25-95%(重量)的具有平均分子量(均数)为至少5000和在主链或侧链上具有聚醚链段的其它化合物Ⅷ,
其中混合物Ⅰa中组合物Ⅱa的重量比例是1-100%(重量)。
6.根据权利要求1-5中任何一项的混合物,其中固体物质Ⅲ是无机碱性化合物,它选自元素周期表Ⅰ、Ⅱ、Ⅲ或Ⅳ主族或Ⅳ副族的元素的氧化物,混合氧化物,硅酸盐,硫酸盐,碳酸盐,磷酸盐,氮化物,氨化物,亚胺化物和碳化物;聚合物,它选自聚乙烯、聚丙烯、聚苯乙烯、聚四氟乙烯、聚偏氟乙烯,聚酰胺,聚酰亚胺;含此类聚合物的固体分散体;和上述两种或多种的组合物。
7.一种复合体,它包括至少一层第一层和至少一层第二层,第一层含导电性电化学活性化合物,第二层不含导电性电化学活性化合物,但含根据权利要求1-6中任何一项的混合物。
8.根据权利要求1-6中任何一项的混合物或权利要求7的复合体在固体电解质、隔板和电极的制备中,和在传感器,电致变色显示窗,显示器,电容器和离子传导膜中的应用。
9.一种固体电解质、隔板、传感器、电致变色显示窗、显示器、电容器和离子传导膜,其各自包含根据权利要求1-6中任何一项的混合物或权利要求7的复合体。
10.一种电化学电池,它包含权利要求9的固体电解质、隔板或电极或其中两种或多种的组合。
11.权利要求10的电化学电池作为汽车电池、仪器电池或扁平电池的应用。
12.具有主要粒度为5纳米-20微米的固体Ⅲ在固体电解质、隔板或电极中以提高电化学电池的周期稳定性的应用。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE19612769.6 | 1996-03-29 | ||
DE19612769A DE19612769A1 (de) | 1996-03-29 | 1996-03-29 | Als Trägermaterial für Festelektrolyten oder Separatoren für elektrochemische Zellen geeignete Gemische |
Publications (2)
Publication Number | Publication Date |
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CN1220030A true CN1220030A (zh) | 1999-06-16 |
CN100470914C CN100470914C (zh) | 2009-03-18 |
Family
ID=7790001
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CNB97194945XA Expired - Fee Related CN100470914C (zh) | 1996-03-29 | 1997-03-27 | 适合作为电化学电池的固体电解质或隔板的组合物 |
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US (3) | US6416905B1 (zh) |
EP (3) | EP1211552A3 (zh) |
JP (1) | JP4110297B2 (zh) |
KR (1) | KR100452076B1 (zh) |
CN (1) | CN100470914C (zh) |
AU (1) | AU2292797A (zh) |
CA (1) | CA2250107C (zh) |
DE (2) | DE19612769A1 (zh) |
ES (1) | ES2178767T3 (zh) |
RU (1) | RU2213395C2 (zh) |
TW (1) | TW355846B (zh) |
WO (1) | WO1997037397A1 (zh) |
ZA (1) | ZA972672B (zh) |
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- 1997-03-27 JP JP53493097A patent/JP4110297B2/ja not_active Expired - Fee Related
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN100334770C (zh) * | 2000-05-24 | 2007-08-29 | 索尼株式会社 | 固体或凝胶电解质和使用该电解质的电池 |
CN102315488A (zh) * | 2011-08-15 | 2012-01-11 | 江苏苏中电池科技发展有限公司 | 聚核硅朊铅酸蓄电池电解液及其制备方法 |
CN105593756A (zh) * | 2014-07-31 | 2016-05-18 | Jsr株式会社 | 显示元件、感光性组合物以及电润湿显示器 |
CN105593756B (zh) * | 2014-07-31 | 2018-06-29 | Jsr株式会社 | 显示元件、感光性组合物以及电润湿显示器 |
Also Published As
Publication number | Publication date |
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US6416905B1 (en) | 2002-07-09 |
JP2000507629A (ja) | 2000-06-20 |
US7118694B2 (en) | 2006-10-10 |
WO1997037397A1 (de) | 1997-10-09 |
RU2213395C2 (ru) | 2003-09-27 |
EP1211552A2 (de) | 2002-06-05 |
DE19612769A1 (de) | 1997-10-02 |
CA2250107A1 (en) | 1997-10-09 |
EP0890196A1 (de) | 1999-01-13 |
US20020160270A1 (en) | 2002-10-31 |
CN100470914C (zh) | 2009-03-18 |
JP4110297B2 (ja) | 2008-07-02 |
US20020155353A1 (en) | 2002-10-24 |
CA2250107C (en) | 2007-06-12 |
EP1209755A2 (de) | 2002-05-29 |
EP0890196B1 (de) | 2002-06-12 |
EP1211552A3 (de) | 2005-11-23 |
KR100452076B1 (ko) | 2004-12-16 |
TW355846B (en) | 1999-04-11 |
ES2178767T3 (es) | 2003-01-01 |
EP1209755A3 (de) | 2005-11-16 |
KR20000005069A (ko) | 2000-01-25 |
DE59707507D1 (de) | 2002-07-18 |
ZA972672B (en) | 1998-09-28 |
AU2292797A (en) | 1997-10-22 |
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