CN1211054A - 用于电容器的电解溶液和电容器 - Google Patents
用于电容器的电解溶液和电容器 Download PDFInfo
- Publication number
- CN1211054A CN1211054A CN98119237A CN98119237A CN1211054A CN 1211054 A CN1211054 A CN 1211054A CN 98119237 A CN98119237 A CN 98119237A CN 98119237 A CN98119237 A CN 98119237A CN 1211054 A CN1211054 A CN 1211054A
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- CN
- China
- Prior art keywords
- capacitor
- electrolytic solution
- nonaqueous electrolyte
- double layer
- electric double
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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Images
Classifications
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
- H01G11/60—Liquid electrolytes characterised by the solvent
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- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
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- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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Abstract
公开了一种用于电容器的非水电解溶液,它释放较少的气体,电化学稳定性的电势窗优良,并且使得电容器具有优良的充电/放电循环性能和安全性能,还公开了含有该非水电解溶液的电容器。该用于电容器的非水电解溶液包括一种含有由上式(Ⅰ)所示的磷酸酯的溶剂和一种电解质。
Description
本发明涉及用于电容器的非水电解溶液,它主要含有磷酸酯,本发明具体是用于电偶层电容器(electric double layer capacitors)的非水电解溶液,更具体的是能量密度高、耐电压性和充电/放电循环性能优良的电容器,尤其是能够形成电偶层电容器的非水电解溶液。
迄今为止,作为集成电路和存储器的备用电源和蓄电池的补充或替代品的电容器,特别是电容介于电池和电容器之间的电偶层电容器,已经被广泛用作低功率直流电源。然而,近年来新型便携式电子设备接踵而至,如配有内置式照相机的VTR,蜂窝式电话和便携式计算机。在这种趋势中,日益增长地需要那些用作备用电源和蓄电池的补充或替代品的电偶层电容器具有更高的能量密度。
与电池不同的是,这些电偶层电容器并非将化学变化转化成电能。它们利用的是电极和电解溶液之间存在的电偶层的大电容来加入或放出电荷,就象电池的充电和放电一样。这些电偶层电容器由两个电极、分隔件和通常是耐腐蚀的电解溶液制成。两个电极由表面积大的材料,如活性炭和粘合剂(如氟树脂)形成,它们通过由聚乙烯或聚丙烯制得的多孔分隔件互相面对面地放置,这两个电极和多孔分隔件之间的空间以及多孔分隔件内部充满着上述电解溶液。
水溶液基电解溶液和有机溶剂基电解溶液(非水电解溶液)用作用于这些电偶层电容器的电解溶液。然而,水溶液基电解溶液的问题是其电化学稳定性的电势窗(potential window)低(约为1.2V),难以得到高能量密度的电偶层电容器。
相反地,与水溶液基电解溶液相比,有机溶剂基电解溶液(非水电解溶液)的电化学稳定性的电势窗高,因此有可能形成高能量密度的电容器。正因为如此,使用非水电解溶液的电偶层电容器正开始迅速地用作非军用电子设备的备用电源。
作为这些非水电解溶液,例如可以使用介电常数高的非水溶剂(如环状碳酸酯)和电解质(如四氟硼酸四乙铵)的混合物。
然而,上述这种电解溶液存在的问题是,由于它们使用环状碳酸酯作为溶剂使得溶剂在高温时脱羧分解,放出大量气体,从而不能得到长寿命的电容器。而且,随着将来电容器的能量密度提高,上述电解溶液电化学稳定性的电势窗可能会不够。正因为如此,希望有一种充电/放电循环性能更好的非水电解质诞生。
本发明的发明人找到了解决上述常规技术中问题的途径。本发明就是要提供用于电容器的非水电解溶液,它释放很少的气体、电化学稳定性的电势窗优良、能使电容器显示优良的充电/放电循环性能和安全性能,本发明还提供含有该非水电解溶液的电容器。
(其中,R1、R2和R3可以相同或不同,是烷基、不饱和烃基或芳基。)
本发明的电容器使用了上述用于电容器的非水电解溶液。
本发明用于电容器的非水电解溶液释放较少气体,电化学稳定性的电势窗高、安全性能和充电/放电循环性能优良。
尤其是将本发明用于电容器的非水电解溶液用于形成电容器时,能够得到产生高电压、释放很少气体、充电/放电循环性能和能量密度优良的电容器。特别是当该电解溶液用于电偶层电容器时,这一效应尤其显著。
图1表示本发明缠绕式(wound-type)电偶层电容器的电容器组件结构的透视图。
图2表示上述电容器组件作为一构件插入金属外壳中与密封件形成整体时的状态的透视图。
以下是本发明非水电解溶液和电容器的具体描述。
用于电容器的非水电解溶液:
本发明用于电容器的非水电解溶液包含一种含有下式(Ⅰ)所示磷酸酯的溶剂和一种电解质。
磷酸酯:
在式(Ⅰ)中,R1、R2和R3可以相同或不同,是烷基、不饱和烃基或芳基。
烷基较好的可以是含1至4个碳原子的基团。烷基的例子包括甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基和叔丁基。
不饱和烃基较好的是含2至4个碳原子的基团。不饱和烃基的例子是乙烯基、烯丙基和异丙烯基。
芳基可以是含6至12个碳原子的基团。芳基的例子包括苯基、苄基、萘基和联苯基。
在本发明的上述式(Ⅰ)中,R1至R3可以相同或不同,较好的是上述烷基或不饱和烃基,R1至R3各自独立,更好的是相同,较好的是选自甲基(-CH3)、乙基(-C2H5)和烯丙基(-CH2-CH=CH2)。
这些磷酸酯具体的例子包括磷酸三甲酯、磷酸三乙酯、磷酸二乙基·甲基酯、磷酸乙基·二甲基酯、磷酸三丙酯、磷酸三丁酯、磷酸三烯丙酯和磷酸烯丙基·二甲基酯。
在本发明中,由上述式(Ⅰ)所示的化合物较好的可以是磷酸三甲酯、磷酸三乙酯和磷酸三烯丙酯,其中式(Ⅰ)中的R1至R3较好的是相同的,选自-CH3、-C2H5和-CH2-CH=CH2。
由上述式(Ⅰ)所示的这些磷酸酯显示了优良的耐酸性,放置在大气中不会氧化,化学稳定而不会在正常的贮存条件下与水反应,也不会与高度反应性的物质(如金属锂)反应。而且,这些磷酸酯具有物理性安全、不易热分解、阻燃和抗电化学氧化或还原的性能。
用于电解溶液的溶剂:
在本发明中,含有所示磷酸酯的溶剂被用作电解溶液的溶剂。这些溶剂可以是上述磷酸酯的至少一种溶剂,或者是与另一种溶剂的混合溶剂。
这另一种溶剂的例子包括环状碳酸酯,如碳酸亚乙酯(1,3-二氧环戊-2-酮)、碳酸亚丙酯(4-甲基-1,3-二氧环戊-2-酮)、碳酸亚丁酯(4,5-二甲基-1,3-二氧环戊-2-酮)和碳酸亚乙烯酯;链状碳酸酯,如碳酸二甲酯、碳酸甲·乙酯、碳酸二乙酯、碳酸甲·丙酯和碳酸甲·异丙酯;环状酯,如γ-丁内酯、3-甲基-γ-丁内酯和2-甲基-γ-丁内酯;链状酯,如甲酸甲酯、甲酸乙酯、乙酸甲酯、乙酸乙酯、乙酸丙酯、丙酸甲酯、丁酸甲酯和戊酸甲酯;环状醚,如1,4-二氧杂环己烷、1,3-二氧戊环、四氢呋喃、2-甲基四氢呋喃和3-甲基-1,3-二氧戊环和2-甲基-1,3-二氧戊环;链状醚,如1,2-二甲氧基乙烷、1,2-二乙氧基乙烷、二乙醚、二甲醚、甲基乙基醚和二丙醚;以及含硫化合物,如四氢噻吩砜。
此外,除了作为例子给出的上述环状碳酸酯之外,日本公开专利平9-63644中所述的含被卤素原子所取代的烷基的环状碳酸酯也可以用作环状碳酸酯。这些环状碳酸酯的例子包括单氟甲基碳酸亚乙酯、二氟甲基碳酸亚乙酯和三氟甲基碳酸亚乙酯(trifluoromethyl-ethylene carbonate)。在这些溶剂中,较好的是环状碳酸酯。
这些溶剂可以单独使用,或者与它们中的一种或不少于两种结合使用。
在本发明中,如果将式(Ⅰ)所示的磷酸酯和另一种溶剂的混合溶剂用作电解溶液的溶剂的话,较好的是由式(Ⅰ)所示的磷酸酯和环状碳酸酯的混合物。在这些用于电解溶液的溶剂中,由式(Ⅰ)所示的磷酸酯的含量较好的是不低于用于电解溶液的溶剂总量的0.1%(重量),特别好的是0.5-100%(重量)。
电解质:
本发明的电容器的非水电解溶液中所含电解质的具体例子包括铵盐,如四氟硼酸四丁铵((C4H9)4NBF4)、四氟硼酸四乙铵((C2H5)4NBF4)、四氟硼酸三乙基一甲基铵((C2H5)3(CH3)NBF4)、六氟磷酸四丁铵((C4H9)4NPF6)、六氟磷酸四乙铵((C2H5)4NPF6)和六氟磷酸三乙基一甲基铵((C2H5)3(CH3)NPF6);鏻盐,如四氟硼酸四丁鏻((C4H9)4PBF4)、四氟硼酸四乙鏻((C2H5)4PBF4)、六氟磷酸四丁鏻((C4H9)4PPF6)、六氟磷酸四乙鏻((C2H5)4PPF6);以及通常用于电偶层电容器的电解溶液的电解质,如国际公开号为WO95/15572的国际申请中所述的电解质。
其中,较好的是使用(C4H9)4NBF4、(C2H5)4NBF4和(C2H5)3(CH3)NBF4。
将上述电解质溶解在上述用于电解溶液的溶剂中,制得本发明的非水电解溶液。在这些用于电容器的非水电解溶液中电解质的含量通常为0.1-3摩尔/升,较好的是0.5-1.5摩尔/升。
由于本发明用于电偶层电容器的非水电解溶液含有式(Ⅰ)所示的磷酸酯,因此该非水电解溶液释放较少的气体、耐电压高、充电/放电循环性能优良。而且,与常规的用于电解溶液的溶剂(如1,3-二氧戊环、四氢呋喃和1,2-二乙氧基乙烯)相比,本发明非水电解溶液的闪点(flash point)高、安全性能优良。而且,使用(C2H5)3(CH3)NBF4使得能得到高的电导率。
正因为如此,使用本发明用于电偶层电容器的非水电解质溶液能够得到释放较少气体、耐电压高和充电/放电循环性能优良的电偶层电容器。
电容器:
电偶层电容器由两个电极、分隔件和通常为耐腐蚀的电解溶液组成。两个电极由表面积大的材料(如活性炭和粘合剂(如氟树脂))形成,它们通过由聚乙烯或聚丙烯制得的多孔分隔件互相面对面地放置,这两个电极和多孔分隔件之间的空间以及多孔分隔件内部充满着电解溶液。
作为电极,较好的是使用由表面积大的材料(如活性炭和粘合剂(如氟树脂))形成的电极。
作为电极材料,活性炭是较好的。活性炭的例子可提及的有多孔活性炭或粉末活性炭,如苯酚基、沥青基、聚丙烯腈基和椰子壳基的活性炭。通常较好的是比表面积不小于1,000米2/克的活性炭。此外,活性炭的制备方法可提及的有蒸气活化法和碱活化法。
粘合剂的例子有羧甲基纤维素、聚偏二氯乙烯、聚乙烯吡咯烷酮、聚酰亚胺、聚乙烯醇和聚丙烯酸。此外,上述电极材料(活性材料)和集电极(collector)结合用于电极通常是较好的。
作为集电极,例如铝箔是较好的。
作为较好的分隔件的例子可提及的有由聚乙烯或聚丙烯制得的多孔膜。
以下通过附图说明电偶层电容器的具体例子。
图1和图2说明了本发明的实施例1和2以及比较例的缠绕式电偶层电容器的电容器组件的结构,以及上述电容器组件作为一构件插入金属外壳中与密封件形成整体时之状态。在图1和图2中,1表示电容器组件,该电容器组件1形成如下:在与阳极端导线2连接的阳极端上缠绕可极化的电极3,在与阴极端导线4连接的阴极端上缠绕可极化的电极5,它们之间放置分隔件6。由橡胶制得的密封件7与电容器组件1的阳极端导线2和阴极端导线4连接。此外,电容器组件1预先经驱动电解溶液(driving electrolytic solution)浸渍,放入由铝制成的有底的圆筒形(bottomed cylindrical form)的金属外壳8中。电容器组件1放入金属外壳8后,将密封件7放在金属外壳8的开口处,通过使金属外壳8经历侧面挤压和卷曲的处理来密封该外壳的开口。结果使得密封件7装入金属外壳8的开口内。
以上说明了缠绕式的电偶层电容器。然而,将本发明电解溶液用于结构不同于缠绕式电偶层电容器的其它电偶层电容器,也可以得到相同的效果。所述其它电偶层电容器例如,日本公开专利平3-51284所述的硬币型(coin type)电偶层电容器和日本公开专利平8-78291所述的层压型电偶层电容器。
在以下实施例中描述了数种较佳实施方案以说明本发明。然而,应该理解本发明并不受到这些具体实施方案的限制。
实施例1
将2.71克(0.0125摩尔)的四氟硼酸四乙铵((C2H5)4NBF4)溶解在磷酸三甲酯中制得25毫升的非水电解溶液,电解质浓度为0.5摩尔/升。测定如此得到的电解溶液的电化学稳定性的电势窗。
额定电容为2.3V30F(18毫米直径×40毫米长度)的如图1所示的缠绕式电偶层电容器制备如下:用如上得到的非水电解溶液作为电解溶液,将表面弄成粗糙的铝箔用椰子壳制成的活性炭末、乙炔黑和羧甲基纤维素的混合粉末在水中的浆液涂覆并干燥,作为可极化的电极,用由聚丙烯制得的非织造的织物作为分隔件。对缠绕式电偶层电容器进行充电/放电试验。
在本发明专利申请中,电解溶液的电化学稳定性的电势窗的评定和充电/放电试验按如下所述进行。
结果见表1。电化学稳定性的电势窗:
将上述电解溶液放入三极、耐电压的测定电池中,该测定电池使用玻璃化炭黑电极作为工作电极和反电极,用Ag/Ag+电极作为参考电极,用电势电流恒定器以10毫伏/秒(mV/sec)对电势进行扫描。Ag/Ag+电极用作参考,不流过不小于1μA的氧化还原分解电流的范围被认为是电化学稳定性的电势窗。充电/放电试验:
充电/放电试验按如下方法进行:在70℃的环境下、以3A的充电电流将电容器充电至最终充电电压为3.5V,然后以3A的放电电流将电容器放电至最终放电电压为1.5V,这一过程定为一个循环。在这些条件下,测定缠绕式电偶层电容器在10,000次循环后的高度(height)的变化量。
实施例2
将2.71克(0.0125摩尔)的四氟硼酸四乙铵((C2H5)4NBF4)溶解在磷酸三甲酯和碳酸亚丙酯以1∶1的重量比混合得到的混合溶剂中,制得25毫升的非水电解溶液,电解质浓度为0.5摩尔/升。以实施例1所述相同的方式测定如此得到的电解溶液的电化学稳定性的电势窗。
以实施例1所述相同的方式,用按实施例2所述制得的非水电解溶液制备额定电容为2.3V30F(18毫米直径×40毫米长度)的缠绕式电偶层电容器。对该缠绕式电偶层电容器进行充电/放电试验。
结果见表1。
实施例3
将2.71克(0.0125摩尔)的四氟硼酸四乙铵((C2H5)4NBF4)溶解在磷酸三烯丙酯中,制得25毫升的非水电解溶液。以实施例1所述相同的方式测定如此得到的电解溶液的电化学稳定性的电势窗。
以实施例1所述相同的方式,用如此制得的非水电解溶液制备额定电容为2.3V30F(18毫米直径×40毫米长度)的缠绕式电偶层电容器。对该缠绕式电偶层电容器进行充电/放电试验。
结果见表1。
实施例4
将2.54克(0.0125摩尔)的四氟硼酸三乙基一甲基铵((C2H5)3(CH3)NBF4)溶解在磷酸三烯丙酯中,制得25毫升的非水电解溶液。以实施例1所述相同的方式测定如此得到的电解溶液的电化学稳定性的电势窗。
以实施例1所述相同的方式,用如此制得的非水电解溶液制备额定电容为2.3V30F(18毫米直径×40毫米长度)的缠绕式电偶层电容器。对该缠绕式电偶层电容器进行充电/放电试验。
结果见表1。
比较例1
按实施例1所述相同的方式制备电解溶液,不同的是用碳酸亚丙酯代替实施例1中的磷酸三甲酯。
以实施例1所述相同的方式,用如此制得的非水电解溶液制备额定电容为2.3V30F(18毫米直径×40毫米长度)的缠绕式电偶层电容器。对该缠绕式电偶层电容器进行充电/放电试验。
结果见表1。
表1
溶剂 | 电解质 | 电化学稳定性的电势窗(对Ag/Ag+的伏特) | 高度的变化量(毫米) | ||
氧化电势 | 还原电势 | ||||
实施例1 | 磷酸三甲酯 | (C2H5)4NBF4 | 1.85 | -2.95 | 0.7 |
实施例2 | 磷酸三乙酯/碳酸亚丙酯(1/1) | (C2H5)4NBF4 | 2.10 | -3.10 | 1.2 |
实施例3 | 磷酸三烯丙酯 | (C2H5)4NBF4 | 4.10 | -2.75 | 0.9 |
实施例4 | 磷酸三甲酯 | (C2H5)3(CH3)NBF4 | 1.86 | -2.95 | 0.7 |
比较例1 | 碳酸亚丙酯 | (C2H5)4NBF4 | 1.75 | -2.90 | 2.0 |
由表1可见,由于与比较例1相比,实施例1、2、3和4的氧化电势和还原电势间的电势差显著,因此实施例1、2、3和4的耐电压高。而且还可以看出,因为与使用比较例1电解溶液的缠绕式电偶层电容器相比,使用实施例1、2、3和4电解溶液的缠绕式电偶层电容器在充电/放电试验后高度只是稍有变化,所以使用本发明的电解溶液能够形成释放较少气体、耐电压高、充电/放电循环性能优良的电偶层电容器。
以上用电偶层电容器作为例子说明了用于电容器的电解溶液。然而,本发明并不限于此,即使是在将该电解溶液用于铝电解电容器的情况下,也可以得到相同的效果。
Claims (8)
2.如权利要求1所述的用于电容器的非水电解溶液,其特征在于上式(Ⅰ)所示的磷酸酯中的R1、R2和R3是含1至4个碳原子的烷基、含2至4个碳原子的不饱和烃基或含6至12个碳原子的芳基。
3.如权利要求1所述的用于电容器的非水电解溶液,其特征在于上式(Ⅰ)所示的磷酸酯中的R1、R2和R3选自CH3、C2H5和CH2-C=CH2。
4.如权利要求1至3中任一项所述的用于电容器的非水电解溶液,其特征在于用于电解溶液的溶剂是上式(Ⅰ)所示的磷酸酯和环状碳酸酯的混合溶剂。
5.一种使用如权利要求1至4中任一项所述的用于电容器的非水电解溶液的电容器。
6.如权利要求5所述的电容器,其特征在于所述电容器是电偶层电容器。
7.一种电偶层电容器,它包含阳极端上的可极化电极、阴极端上的可极化电极、分隔件和电解溶液,其特征在于所述可极化电极是用活性炭末作为电极材料的电极,所述电解溶液是如权利要求1至4中任一项所述的电解溶液。
8.如权利要求7所述的电偶层电容器,其特征在于所述可极化电极是在集电极箔上涂覆加入了乙炔黑和羧甲基纤维素的活性炭末的混合粉末并干燥而得到的电极。
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JP247144/1997 | 1997-09-11 | ||
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JP24714497A JP3793905B2 (ja) | 1997-09-11 | 1997-09-11 | 電気二重層コンデンサ用非水電解液および非水電気二重層コンデンサ |
JP356882/97 | 1997-12-25 | ||
JP356882/1997 | 1997-12-25 | ||
JP9356882A JPH11238652A (ja) | 1997-12-25 | 1997-12-25 | 電気二重層コンデンサ用非水電解液および非水電気二重層コンデンサ |
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EP (1) | EP0902446A3 (zh) |
KR (1) | KR19990029687A (zh) |
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CN100334771C (zh) * | 2002-10-22 | 2007-08-29 | 三菱化学株式会社 | 非水电解质溶液和使用它的非水电解质溶液二次电池 |
CN100408634C (zh) * | 2005-03-23 | 2008-08-06 | 三洋电机株式会社 | 燃料电池用电解质、膜电极接合体以及燃料电池用电解质的制造方法 |
CN106449104A (zh) * | 2016-09-27 | 2017-02-22 | 江苏国泰超威新材料有限公司 | 一种阻燃型铝电解电容器用电解液 |
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JP4257725B2 (ja) * | 2001-03-30 | 2009-04-22 | 株式会社ブリヂストン | 非水電解液二次電池 |
JP4004769B2 (ja) * | 2001-10-17 | 2007-11-07 | Necトーキン株式会社 | 電解液、並びにこれを用いた電気化学セル |
JP4379156B2 (ja) * | 2004-03-03 | 2009-12-09 | パナソニック株式会社 | アルミ電解コンデンサ |
US7833660B1 (en) | 2006-09-07 | 2010-11-16 | The United States Of America As Represented By The Secretary Of The Army | Fluorohaloborate salts, synthesis and use thereof |
US7820323B1 (en) | 2006-09-07 | 2010-10-26 | The United States Of America As Represented By The Secretary Of The Army | Metal borate synthesis process |
US20080137265A1 (en) * | 2006-12-12 | 2008-06-12 | Venkateswaran Sagar N | High voltage non-toxic electrolytes for ultracapacitors |
EP2884511B1 (en) * | 2012-08-10 | 2019-06-26 | Nippon Chemi-Con Corporation | Flame-retardant electrolytic capacitor |
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JPS6023973A (ja) | 1983-07-15 | 1985-02-06 | Hitachi Maxell Ltd | 有機電解質電池 |
JP2611262B2 (ja) | 1987-10-08 | 1997-05-21 | 三菱化学株式会社 | 難燃性電解コンデンサ |
EP0449145B1 (en) * | 1990-03-29 | 1998-01-28 | Matsushita Electric Industrial Co., Ltd. | Electric double layer capacitor and method for producing the same |
JP3131905B2 (ja) | 1990-11-19 | 2001-02-05 | 三菱化学株式会社 | リチウム電池用電解液の難燃化剤 |
JP3387144B2 (ja) * | 1993-03-30 | 2003-03-17 | 三菱化学株式会社 | 電解コンデンサ用電解液 |
EP0684620B1 (en) * | 1993-12-03 | 2003-06-04 | Sanyo Chemical Industries, Ltd. | Electrolytic solution and electrochemical element prepared therefrom |
US5580684A (en) * | 1994-07-07 | 1996-12-03 | Mitsui Petrochemical Industries, Ltd. | Non-aqueous electrolytic solutions and non-aqueous electrolyte cells comprising the same |
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CN100334771C (zh) * | 2002-10-22 | 2007-08-29 | 三菱化学株式会社 | 非水电解质溶液和使用它的非水电解质溶液二次电池 |
CN100408634C (zh) * | 2005-03-23 | 2008-08-06 | 三洋电机株式会社 | 燃料电池用电解质、膜电极接合体以及燃料电池用电解质的制造方法 |
CN106449104A (zh) * | 2016-09-27 | 2017-02-22 | 江苏国泰超威新材料有限公司 | 一种阻燃型铝电解电容器用电解液 |
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EP0902446A2 (en) | 1999-03-17 |
US6185089B1 (en) | 2001-02-06 |
KR19990029687A (ko) | 1999-04-26 |
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CN1154133C (zh) | 2004-06-16 |
TW403922B (en) | 2000-09-01 |
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