CN104051159A - 用于高温环境的湿式电解电容器 - Google Patents
用于高温环境的湿式电解电容器 Download PDFInfo
- Publication number
- CN104051159A CN104051159A CN201410078762.3A CN201410078762A CN104051159A CN 104051159 A CN104051159 A CN 104051159A CN 201410078762 A CN201410078762 A CN 201410078762A CN 104051159 A CN104051159 A CN 104051159A
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- Prior art keywords
- anode
- electrolytic capacitor
- wet electrolytic
- acid
- seal
- Prior art date
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Classifications
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- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/145—Liquid electrolytic capacitors
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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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- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
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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
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- H—ELECTRICITY
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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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- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明公开了一种湿式电解电容器,其包括由阳极氧化的烧结多孔体形成的阳极及液体工作电解质。外壳包含一涂覆有电化学活性材料的金属基体。通过与电容器构造和密封组件相关的特征的独特和受控的组合,本发明者发现,可以在较高温度下实现良好的电气性质(例如,ESR稳定性)。湿式电解电容器有助于实现这样良好的ESR稳定性的一个独特的特征是在阴极的金属基体上存在在受控厚度范围内的介电层。在其他实施方案中,可采用密封组件,其包含一密封件(例如,玻璃-金属密封件)和一弹性隔障密封件,该弹性隔障密封件由高温弹性材料形成。
Description
技术领域
本发明涉及一种湿式电解电容器,特别是一种用于高温环境的湿式电解电容器。
背景技术
一般而言,与某些其它类型的电容器相比,电解电容器每单位体积的电容更大,使其在较高电流和低频率电路中很有价值。已开发出一种类型的电容器,其为一包含烧结钽粉阳极的“湿式”电解电容器。这些钽“金属块(slug)”具有非常大的内部表面积。这些钽金属块首先经历电化学氧化,形成一氧化层涂层作为电介质覆盖钽主体的整个外部和内部表面。然后将阳极化的钽金属块密封在包含高导电性和一般腐蚀性液体电解液的容器(can)中,该容器具有高表面积和导电衬里,能使电流流到液体电解液。可惜的是,这种湿式电容器在液体电解液泄漏时会出现问题。例如,在运作过程中会放出气体(如氢气),导致电容器内的压力增加。这可导致泄漏发生在传统非密封式聚合物密封件周围,端线从电容器外壳突出的地方。
鉴于上述情况,人们通常采用气密密封件(例如,玻璃-金属密封),端线可安全地延伸穿过该密封件。但是,密封件本身有时会被液体电解液腐蚀。由于这个原因,人们也通常采用液体密封件以防止密封件的内区域暴露于电解液。例如,Knight等人的专利号为7,206,186的美国专利介绍了一液体密封,其通过压缩盖子下侧和连接到电容器元件的端板之间的弹性环形成。也可将衬套放置在弹性环内,以相对于密封件使该环居中。尽管人们作出种种努力来改善这种电解电容器的液体密封,但问题仍然存在。例如,即使在使用了液体密封件的情况下,本发明者发现,这种电容器在与许多商业应用相关的高温环境中仍倾向于表现出不良的等效串联电阻(“ESR”)稳定性。
因此,仍然需要一改进的密封的湿式电解电容器。
发明内容
本发明的一个实施方案公开了一种湿式电解电容器,其包括一外壳,该外壳限定了一开口和一包围内部的侧壁,其中该外壳包含一用电化学活性材料涂覆的金属基体;设置在外壳内部的阳极,其中阳极由一阳极氧化的烧结的多孔主体形成,该阳极包括一从中延伸的阳极引线;以及一液体工作电解液,该电解液与阳极和电化学活性材料电接触。用2伏特偏压和1伏特信号在120Hz的频率下测量,该湿式电解电容器在200℃的温度下表现出约3000毫欧姆或以下的等效串联电阻。
本发明的另一个实施方案公开了一种湿式电解电容器,其包括一外壳,该外壳限定了一开口和一包围内部的侧壁,其中该外壳包含一阳极氧化的金属基体,该基体具有厚度约10纳米至约500纳米的介电层;设置在外壳内部的阳极,其中阳极由一阳极氧化的烧结的多孔主体形成,该阳极包括一从中延伸的阳极引线;以及一液体工作电解液,该电解液与阳极和电化学活性材料电接触。
本发明的又一个实施方案公开了一种湿式电解电容器,其包括一个外壳,其限定了一开口和一包围内部的侧壁,其中该外壳包含一用电化学活性材料涂覆的金属基体;设置在外壳内部的阳极,其中该阳极由一阳极氧化的烧结的多孔主体形成,该阳极包括一从中延伸的阳极引线;液体工作电解液,该电解液与阳极和电化学活性材料电接触;以及覆盖外壳的开口的密封组件,其包含密封件(hermetic seal)和隔障密封件,其中隔障密封件包含一弹性材料,按照ASTM D412进行测定,在500毫米每分钟的拉伸夹头速度(tensile grip speed),在200℃的温度下,该弹性材料展示出在断裂时约100%或以上的伸长率和/或在断裂时约2兆帕斯卡或以上的拉伸强度。
本发明的另一个实施方案公开了一种形成电解电容器的方法。该方法包括:通过阳极氧化一金属基体,以在其上形成厚度约10纳米至约500纳米的介电层,然后用电化学活性材料涂覆基体,形成一外壳;将阳极放置在外壳的内部,其中阳极由阳极氧化的烧结的多孔主体形成,所述阳极包含一从中延伸的阳极引线;以及放置一与阳极和电化学活性材料电接触的液体工作电解质。
本发明的其它特点和方面将在下文进行更详细的说明。
附图说明
本发明完整的和能够实现的公开内容,包括对于本领域技术人员而言的最佳方式,将参考附图在说明书的其余部分中更具体地给出,其中:
图1是本发明湿式电解电容器的一个实施方案的示意图;
图2是显示实施方案1的电容器在200℃下的ESR(欧姆)相对于时间(小时)的图形化结果;以及
图3是显示实施方案2的电容器在200℃下的ESR(欧姆)相对于时间(小时)的图形化结果。
说明书和附图中重复使用的附图标记意在表示相同或者相似的本发明的特征或元件。
具体实施方式
本领域技术人员应当理解,目前的讨论仅作为示范性实施方案的描述,并不是对本发明更广泛范围的限制。
一般来说,本发明针对一湿式电解电容器,其包含一阳极和一液体工作电解液,该阳极由阳极氧化的烧结的多孔主体形成,该液体工作电解液置于外壳内。该外壳包含一涂覆有电化学活性材料的金属基体。通过与电容器构造和密封组件相关的特征的独特和受控的组合,本发明者发现,可以在较高温度下实现良好的电气性质(例如,ESR稳定性)。例如,在频率120Hz,偏压2伏特和1伏特信号下测量时,本发明电容器的ESR可为约3,000毫欧或以下,在一些实施方案中,低于约2,000毫欧,在一些实施方案中,为约1至约1,000毫欧,以及在一些实施方案中,为约50毫欧至约800毫欧。值得注意的是,这样低的ESR值甚至在高温下仍可维持。例如,该值可维持在约150℃到约400℃的温度范围内,在一些实施方案中,维持在约175℃到约350℃,以及在一些实施方案中,维持在约200℃到约300℃(例如,200℃、225℃、250℃、275℃或300℃)。该值的工作时间也可维持较长,如约100小时或更长,在一些实施方案中,维持约200小时至约3000小时,以及在一些实施方案中,维持约400小时至约2000小时(例如,500小时、600小时、700小时、800小时、900小时、1000小时、1100小时、1200小时或2000小时)。
湿式电解电容器有助于实现这样良好的ESR稳定性的一个独特的特征是在阴极的金属基体上存在在受控厚度范围内的介电层。例如,厚度可为约10纳米至约500纳米,在一些实施方案中为约15纳米至约200纳米,在一些实施方案中为约20纳米至约100纳米,以及在一些实施方案中为约30纳米至约80纳米。在受理论限制的范围内,人们相信,通常存在于工作电解液中的酸可在较高温度下与金属基体(例如,钽)经历二次反应。因此,较厚介电层的存在可有助于使金属基体钝化,并从而减少工作电解液与基体反应的可能性,以降低其导电率并增加ESR。但是,通过确保厚度控制在上述范围内,本发明者还发现,阴极的导电率并未降低至对电容器的电气性质造成不利影响的程度。
当然,也可以选择电容器的其它方面来帮助实现高温下需要的性能。在某些实施方案中,例如,可采用密封组件,其包含一密封件(例如,玻璃-金属密封件)和一弹性隔障密封件,该弹性隔障密封胶由高温弹性材料形成。通过有选择地控制弹性材料的性质,本发明者发现,所得隔障密封件甚至可在高温下维持其弹性。这为隔障密封件提供了抑制从电解质泄漏的蒸汽逃逸出电容器的能力,否则会造成ESR快速增加。隔障密封件还可具有其余的益处,其可限制使用过程中阳极的振动,这种益处可增加机械稳定性。
下面将更为详细地说明本发明的多种实施方案。
I.阴极
该电容器的阴极通常包含一金属基体,金属基体表面涂覆有一电化学活性材料。该金属基体可以由多种不同的金属形成,例如钽、铌、铝、镍、铪、钛、铜、银、钢(如不锈钢),它们的合金,它们的复合物(如涂覆导电氧化物的金属)等。钽尤其适合用于本发明。如本领域技术人员熟知的,基体的几何构造通常可以不同,例如形式为箔、片、筛、容器、罐等。金属基体可形成整个或部分电容器外壳,或简单地应用到外壳上。不管怎样,基体可具有多种形状,如一般圆柱形、D形、矩形、三角形、棱形等。如果需要,可对基体的表面进行粗化处理以增加其表面积和增加材料能粘附其上的程度。例如,在一个实施方案中,对金属基体表面进行化学蚀刻,如在表面涂上腐蚀性物质的溶液(如盐酸)。也可以采用机械粗化。例如,可通过向至少部分基体表面上喷射一股磨料(如沙)而对基体表面进行喷砂处理。
不论其性质如何,金属基体的表面(如内表面)可能会接受一电压以引起如上文所述的氧化膜(介电层)的阳极形成(“阳极氧化”)。例如,钽(Ta)基体可经阳极氧化以形成五氧化二钽(Ta2O5)的介电层。阳极氧化可首先通过在金属基体上施加一电解质,例如将基体浸到含电解质的槽中,然后施加一电流。电解质通常为液体,如溶液(如水溶液或非水溶液)、分散体、熔体等。电解质中通常使用溶剂,如水(如去离子水);醚(如二乙醚和四氢呋喃);醇(如甲醇、乙醇、正丙醇、异丙醇和丁醇);甘油三酯;酮(例如,丙酮、甲基乙基酮和甲基异丁基酮);酯(例如,乙酸乙酯、醋酸丁酯、二乙二醇乙醚乙酸酯、和甲基丙醇乙酸酯);酰胺(例如,二甲基甲酰胺、二甲基乙酰胺、二甲基辛/癸脂肪酸酰胺和N-烷基吡咯烷酮);腈(如乙腈、丙腈、丁腈和苄腈);亚砜或砜(例如,二甲亚砜(DMSO)和环丁砜);等等。溶剂占电解质的大约50wt.%-大约99.9wt.%,在一些实施方案中占大约75wt.%-大约99wt.%,以及在一些实施方案中占大约80wt.%-大约95wt.%。虽然并不要求,但是,为了利于形成氧化物,通常使用含水溶剂(如水)。事实上,水在电解质所用溶剂中的含量是大约1wt.%或更高,在一些实施方案中是大约10wt.%或更高,在一些实施方案中是大约50wt.%或更高,在一些实施方案中,是大约70wt.%或更高,以及在一些实施方案中,是大约90wt.%至100wt.%。
电解质是导电性的,并且其在温度25℃下测定的导电率为大约1毫西门子每厘米(“mS/cm”)或以上,在一些实施方案中,为大约30mS/cm或以上,以及在一些实施方案中,为大约40mS/cm到大约100mS/cm。为增加电解质的导电性,可采用能够在溶剂中离解成离子的化合物。适用于此目的的合适的离子化合物包括,例如,酸,如盐酸、硝酸、硫酸、磷酸、多磷酸、硼酸、有机硼酸(boronic acid)等;有机酸,包括羧酸,如丙烯酸、甲基丙烯酸、丙二酸、琥珀酸、水杨酸、磺基水杨酸、己二酸、马来酸、苹果酸、油酸、五倍子酸、酒石酸、柠檬酸、甲酸、乙酸、乙醇酸、草酸、丙酸、邻苯二甲酸、间苯二甲酸、戊二酸、葡糖酸、乳酸、天冬氨酸、谷氨酸、衣康酸、三氟乙酸、巴比妥酸、肉桂酸、苯甲酸、4-羟基苯甲酸、氨基苯甲酸等;磺酸,例如甲磺酸、苯磺酸、甲苯磺酸、三氟甲磺酸、苯乙烯磺酸、萘二磺酸、羟基苯磺酸、十二烷基磺酸、十二烷基苯磺酸等;高分子酸,例如,聚(丙烯酸)或聚(甲基丙烯酸)及其共聚物(例如,马来酸-丙烯酸共聚物、磺酸-丙烯酸共聚物、苯乙烯-丙烯酸共聚物)、角叉菜酸、羧甲基纤维素、藻酸等。选择离子化合物的浓度,以获得要求的导电率。例如,酸(如磷酸)可占电解质的大约0.01wt.%-大约5wt.%,在一些实施方案中占大约0.05wt.%-大约0.8wt.%,以及在一些实施方案中占大约0.1wt.%-大约0.5wt.%。如果需要的话,电解质中还可以使用离子化合物的共混物。
使电流通过电解质,形成介电层。电压值控制电荷(电流乘以时间),并从而控制介电质层的厚度。例如,一开始可以恒电流模式建立电源供应,直到达到要求的电压。然后,可将电源供应切换到电压保持恒定的恒电位模式,以确保在金属基体表面形成要求厚度的电介质。当然,也可以采用人们熟悉的其它方法,如脉冲法。不管怎样,要有助于达到如上文所述的所需厚度的介电层,阳极氧化过程中使用的形成电压(通常等于峰电压)通常很高,例如约5伏特或以上,在一些实施方案中约7伏特或以上,在一些实施方案中为约10伏特至约25伏特,以及在一些实施方案中,为约12至约22伏特。电压水平可变化(例如不断增加),或在这个范围内保持恒定。阳极氧化溶液的温度范围可为约10℃至约200℃,在一些实施方案中为约20℃至约150℃,以及在一些实施方案中,为约30℃至约100℃。所得介电层因此可如上所述在金属基体表面上形成。
一旦形成,就往阳极氧化的金属基体上施加电化学活性材料以增加电解质与基体进行电化学通讯的有效表面积。在给定尺寸时,这种增加的有效表面积可以使形成的电容器的阴极电容增加,和/或在给定电容时,这种增加的有效表面积可以减小电容器的尺寸。电化学活性材料的性质可不同。例如,可采用一特定的材料,其包含导电颗粒,例如由以下形成的导电颗粒:钌、铱、镍、铑、铼、钴、钨、锰、钽、铌、钼、铅、钛、铂、钯和锇以及这些金属的组合。还可采用非绝缘氧化物导电颗粒。合适的氧化物可包含一金属,该金属选自钌、铱、镍、铑、铼、钴、钨、锰、钽、铌、钼、铅、钛、铂、钯和锇以及这些金属的组合。尤其合适的金属氧化物包括二氧化钌、氧化铌、二氧化铌、氧化铱和二氧化锰。还可采用具有所需导电性的含碳颗粒,例如活性碳、炭黑、石墨等。活性碳的一些合适的形式以及其形成技术描述于Ivey等人的专利号为5,726,118的美国专利以及Wellen等人的专利号为5,858,911的美国专利。钽颗粒可特别适合用作电化学活性材料。
如果需要,可将电化学活性颗粒(例如,钽颗粒)烧结以形成多孔的整块物质。例如,烧结可在从大约800℃到大约2000℃温度下进行,在一些实施方案中,从大约1200℃到大约1800℃,以及在一些实施方案中,从大约1500℃到大约1700℃,烧结时间为从大约5分钟到大约100分钟,以及在一些实施方案中,为从大约10分钟到大约50分钟。这可在一个或多个步骤中进行。如果需要,烧结可在还原性气氛下进行,例如真空、惰性气体、氢气等。还原性气氛的压力可从大约10托至大约2000托,在一些实施方案中,从大约100托至大约1000托,以及在一些实施方案中,从大约100托至大约930托。也可以使用氢气和其它气体(如氩气或氮气)的混合物。
还可采用导电聚合物涂层作为电化学活性材料。在阴极不使用电线组件的那些实施方案中,这种涂层特别合适。导电聚合物的涂覆层可由一层或多层形成。这些涂层采用的材料可有所不同。例如,在一个实施方案中,所述材料包括通常是π-共轭的,并且氧化或还原后具有导电性的导电聚合物。此类π-共轭的导电聚合物的实例包括,例如,聚杂环类(例如聚吡咯;聚噻吩、聚苯胺等)、聚乙炔、聚-对苯撑、聚苯酚盐等。取代聚噻吩特别适合用作导电聚合物,因为其具有特别良好的机械强度和电气性能。在一个具体实施方案中,取代聚噻吩具有下述通式结构:
其中,
T是O或S;
D是任选取代C1-C5烯烃基(例如,亚甲基、乙烯基、正丙烯基、正丁烯基、正戊烯基等);
R7是线性或支链的任选取代C1-C18烷基(例如,甲基、乙基、正丙基或异丙基、正丁基、异丁基、仲丁基或叔丁基、正戊基、1-甲基丁基、2-甲基丁基、3-甲基丁基、1-乙基丙基、1,1-二甲基丙基、1,2-二甲基丙基、2,2-二甲基丙基、正己基、正庚基、正辛基、2-乙基己基、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、正十六烷基、正十八烷基等);任选取代C5-C12环烷基(如环戊基、环己基、环庚基、环辛基、环壬基、环癸基等);任选取代C6-C14芳基(如苯基、萘基等);任选取代C7-C18芳烷基(如苄基、邻、间、对-甲苯基、2,3-、2,4-、2,5-、2,6-、3,4-、3,5-二甲苯基、三甲苯基等);任选取代C1-C4羟烷基或羟基;及
q是0-8的整数,在一些实施方案中,是0-2的整数,以及在一个实施方案中,是0;及
n是2-5000,在一些实施方案中,n是4-2000,在一些实施方案中,n是5-1000。“D”或“R7”的取代基实例包括,例如,烷基、环烷基、芳基、芳烷基、烷氧基、卤基、醚、硫醚、二硫化物、亚砜、砜、磺酸酯、氨基、醛、酮、羧酸酯、羧酸、碳酸酯、羧化物、氰基、烷基硅烷和烷氧基硅烷基、羧酰胺基等。
尤其适合的噻吩聚合物是“D”为任选取代C2-C3烯烃基的噻吩聚合物。例如,聚合物可为具有下述通式结构的任选取代聚(3,4-乙烯基二氧噻吩):
形成例如上文所述导电聚合物的方法是本领域所熟知的。例如,Merker等人的美国专利申请6,987,663介绍了从单体前体形成取代聚噻吩的各种技术。例如,单体前体可具有以下结构:
其中,
T、D、R7和q定义如上文定义。尤其适合的噻吩单体是其中“D”为任选取代C2-C3烯基的噻吩单体。例如,可以使用具有下述通式结构的任选取代3,4-烯烃基二氧噻吩:
其中,R7和q如上文所定义。在一个具体的实施方案中,“q”是0。3,4-乙烯基二氧噻吩的一个市售合适的实例可从Heraeus Clevios的名称为CleviosTMM获得。其它合适的单体也描述于Blohm等人的专利号为5,111,327和Groenendaal等人的专利号为6,635,729的美国专利中。也可以采用这些单体的衍生物,例如上述单体的二聚体或三聚体。分子量更高的衍生物,即,单体的四聚体、五聚体等也适合用于本发明。衍生物可以由相同的或不同的单体单元构成,可以以纯物质形式使用及以相互混合的混合物使用和/或与单体混合的混合物使用。还可以使用这些前体的氧化形式或还原形式。
在氧化催化剂存在下,噻吩单体可进行化学聚合。氧化催化剂通常包含一过渡金属阳离子,如铁(III)、铜(II)、铬(VI)、铈(IV)、锰(IV)、锰(VII)、钌(III)阳离子等。还可用掺杂物为导电聚合物提供过量电荷和稳定聚合物的导电性。掺杂物一般包括无机或有机阴离子,如磺酸离子。在某些实施方案中,前体溶液中使用的氧化催化剂包括阳离子(如过渡金属)和阴离子(如磺酸),从而兼具催化作用和掺杂功能。例如,氧化催化剂可以是过渡金属盐,包括铁(III)阳离子,如卤化铁(III)(如FeCl3)或其它无机酸的铁盐(III),如Fe(ClO4)3或Fe2(SO4)3及有机酸铁盐(III)和包含有机自由基的无机酸的铁盐(III)。带有机基团的无机酸的铁(III)盐实例包括,例如,C1–C20烷醇的硫酸单酯铁(III)盐(如月桂基硫酸铁(III)盐)。同样,有机酸铁(Ⅲ)盐实例包括,例如,C1-C20烷基磺酸铁(Ⅲ)盐(例如,甲烷磺酸、乙烷磺酸、丙烷磺酸、丁烷磺酸或十二烷基磺酸);脂肪族全氟磺酸铁(Ⅲ)盐(如三氟甲烷磺酸、全氟丁烷磺酸或全氟辛烷磺酸);脂肪族C1-C20羧酸铁(Ⅲ)盐(如2-乙基己基羧酸);脂肪族全氟羧酸铁(Ⅲ)盐(如三氟乙酸或全氟辛酸);任选被C1-C20烷基取代的芳香族磺酸铁(Ⅲ)盐(如苯磺酸、邻-甲苯磺酸、对-甲苯磺酸或十二烷基苯磺酸);环烷烃磺酸铁(Ⅲ)盐(如樟脑磺酸)等。也可以使用上文提到的铁(III)盐的混合物。对甲苯磺酸铁(III)和邻甲苯磺酸铁(III)及其混合物,尤其适合本发明。一种商业合适的邻-甲苯磺酸铁(III)盐是H.C.Starck GmbH以名称CleviosTMC销售的产品。
可以采用各种方法形成导电聚合物涂层。在一个实施方案中,氧化催化剂和单体按顺序或者一起施加,使聚合反应在基体上原位进行。合适的用于形成导电聚合物涂层的施加技术包括丝网印刷、浸渍、电泳涂覆和喷涂等。例如,一开始单体可以与氧化催化剂混合,以形成前体溶液。一旦形成混合物,即可将其施加到基体上,然后让其聚合,从而在表面上形成导电涂层。或者,可以按顺序施加氧化催化剂和单体。例如,在一个实施方案中,可将氧化催化剂溶解在有机溶剂(例如,丁醇)中,然后作为浸渍溶液施加。接着,干燥基体,以除去其中的溶剂。然后,将基体浸到包含单体的溶液中。根据使用的氧化剂和要求的反应时间,聚合通常在温度为大约-10℃到大约250℃下进行,在一些实施方案中,从大约0℃到大约200℃下进行。合适的聚合技术,如上文所述的那些技术,在Biler的美国专利7,515,396中进行了更为详细的描述。施加此类导电涂层的其它方法在Sakata等人的美国专利5,457,862、Sakata等人的美国专利5,473,503、Sakata等人的美国专利5,729,428及Kudoh等人的美国专利申请5,812,367中有所描述。
除原位涂覆外,导电聚合物层还可以采用导电聚合物颗粒分散体的形式施加。虽然它们的大小可不同,但是,一般要求颗粒具有小的直径,以增加可粘附到基体上的表面积。例如,颗粒的平均粒径可为大约1到大约500纳米,在一些实施方案中,从大约5到大约400纳米,以及在一些实施方案中,从大约10到大约300纳米。颗粒的D90值(粒径小于或等于D90值的颗粒占所有固体颗粒总体积的90%)可为大约15微米或更小,在一些实施方案中为大约10微米或更小,以及在一些实施方案中为大约1纳米到大约8微米。颗粒的直径可采用已知的技术测定,如超速离心法、激光衍射法等。
电化学活性涂层的总目标厚度通常根据电容器要求的性质而变化。通常,涂层的厚度为约0.2微米(“μm”)至约50μm,在一些实施方案中为约0.5μm至约20μm,以及在一些实施方案中,为约1μm至约5μm。不管怎样,所得的阴极,包括基体、电化学活性材料和任选的电线组件,可具有较小的厚度。例如,阴极可具有的厚度范围为约50毫米至约2000毫米,在一些实施方案中为约100毫米至约1500毫米,以及在一些实施方案中,为约200毫米至约1000毫米。
II.阳极
电解电容器的阳极包括由阀金属组分形成的多孔阳主体。阀金属组分包含一阀金属(即能够氧化的金属)或基于阀金属的化合物,如钽、铌、铝、铪、钛及它们的合金、它们的氧化物、它们的氮化物等。例如,阀金属组分可以包含一铌的导电氧化物,如铌氧原子比为1:1.0±1.0的铌的氧化物,在一些实施方案中,铌氧原子比为1:1.0±0.3,在一些实施方案中,铌氧原子比为1:1.0±0.1,以及在一些实施方案中,铌氧原子比为1:1.0±0.05。例如,铌的氧化物可以是NbO0.7、NbO1.0、NbO1.1和NbO2。这些阀金属氧化物的实例在Fife美国专利6,322,912、Fife等人的美国专利6,391,275、Fife等人的美国专利6,416,730、Fife的美国专利6,527,937、Kimmel等人的美国专利6,576,099、Fife等人的美国专利6,592,740、Kimmel等人的美国专利6,639,787、Kimmel等人的美国专利7,220,397,及Schnitter的美国专利申请公布2005/0019581、Schnitter等人的美国专利申请公布2005/0103638及Thomas等人的美国专利申请公布2005/0013765中均有所描述,以上所有文献通过引用以全文的形式引入本文中用于所有目的。
为了形成阳极,通常使用阀金属组分粉末。所述粉末可包含多种的任何形状的颗粒,如结节状的、角状的、片状的等,及它们的混合物。尤其适合的粉末是Cabot Corp.(如C255片状粉末、TU4D片状/结节状粉末等)及H.C.Starck(例如NH175结节状粉末)供应的钽粉。。可使用本领域技术人员所熟知的技术来形成所述粉末。例如,前体钽粉可以通过使用还原剂(例如氢、钠、钾、镁、钙等)还原钽盐(例如,氟钽酸钾(K2TaF7)、氟钽酸钠(Na2TaF7)、五氯化钽(TaCl5)等)来形成。在本发明中可以利用多种的任何的粉碎技术来获得所需的颗粒特性。例如,可以将粉末分散到液体介质(例如乙醇、甲醇、氟化的液体等)中以形成浆。接着,可以在磨粉机(mill)中将浆与研磨介质(例如,金属球,如钽)混合。研磨介质的数量可有所不同,这通常取决于磨粉机的大小,例如从大约100到大约2000,以及在一些实施方案中,从大约600至大约1000。起始粉末、液体介质和研磨介质可以任何比例混合。例如,初始阀金属粉末和研磨介质的比可从大约1:5到大约1:50。同样地,液体介质的体积和混合的初始阀金属粉末的体积比可从约0.5:1到约3:1,在一些实施方案中,从约0.5:1到约2:1,以及在一些实施方案中,从约0.5:1到约1:1。本发明可使用的磨粉机的一些实例在美国专利5,522,558、5,232,169、6,126,097和6,145,765中有所描述。
研磨可进行任何预定量的时间以获得目标特定表面积。例如,研磨时间的范围从约30分钟至约40分钟,在一些实施方案中,从约1小时至约20小时,以及在一些实施方案中,从约5小时至约15小时。研磨可在任何所需的温度进行,包括室温或高温。研磨后,可例如通过空气干燥、加热、过滤、蒸发等将液体介质与粉末分离或从粉末中除去。例如,可选地可使粉末经历一个或多个酸浸步骤以除去金属杂质。这种酸浸步骤是业内所熟知的工艺,并且可采用多种任何的酸,如矿物酸(如盐酸、氢溴酸、氟氢酸、磷酸、硫酸、硝酸等)、有机酸(如柠檬酸、酒石酸、甲酸、草酸、苯甲酸、丙二酸、琥珀酸、己二酸、邻苯二甲酸等)等等。
尽管不要求,但是可使用业内所知的任何技术来使粉末凝聚(agglomerate)。可以多种方法凝聚这种粉末,例如通过一个或多个加热处理步骤,加热温度从大约700℃到大约1400℃,在一些实施方案中,从大约750℃到大约1200℃,以及在一些实施方案中,从大约800℃到大约1100℃。加热处理可在惰性或还原性气氛中进行。例如,加热处理可在包含氢或释放氢的化合物(例如,氯化铵、氢化钙、二氢化镁等)的气氛中进行,以部分烧结粉末和减少杂质(例如,氟)的含量。如果需要,凝聚也可以在吸气材料(getter material)如镁存在的时候进行。热处理后,可通过逐步通入空气来钝化颗粒。其他合适的凝聚技术也在Rao的美国专利6,576,038、Wolf等人的美国专利6,238,456、Pathare等人的美国专利5,954,856、Rerat的美国专利5,082,491、Getz的美国专利4,555,268、Albrecht等人的美国专利4,483,819、Getz等人的美国专利4,441,927和Bates等人的美国专利4,017,302中有所描述。
粉末中也可加入某些额外的组分。例如,粉末可任选与粘结剂(binder)和/或润滑剂混合,以保证在压制时颗粒彼此充分地粘结在一起。合适的粘结剂实例包括,例如,聚(乙烯醇缩丁醛);聚乙酸乙烯酯;聚乙烯醇;聚乙烯吡咯烷酮;纤维素聚合物,如羧甲基纤维素、甲基纤维素、乙基纤维素、羟乙基纤维素和甲基羟乙基纤维素;无规聚丙烯,聚乙烯;聚乙二醇(如Dow Chemical Co.,(陶氏化学公司)的CarbowaxTM);聚苯乙烯、聚(丁二烯/苯乙烯);聚酰胺、聚酰亚胺和聚丙烯酰胺,高分子量聚醚;环氧乙烷和环氧丙烷的共聚物;氟聚合物,如聚四氟乙烯、聚偏二氟乙烯和氟-烯烃共聚物;丙烯酸聚合物,如聚丙烯酸钠、聚(低烷基丙烯酸酯)、聚(低烷基甲基丙烯酸酯)及低烷基丙烯酸酯和甲基丙烯酸酯的共聚物;和脂肪酸及蜡,如硬脂酸和其他皂质脂肪酸、植物蜡、微晶蜡(精制石蜡)等。可将粘结剂溶解和分散于溶剂中。示例性溶剂可包括水、醇等。使用时,粘结剂和/或润滑剂的百分含量是总物质重量的大约0.1%-大约8%。然而,应该理解的是,本发明并不要求必须使用粘结剂和/或润滑剂。
得到的粉末可以采用任常规的粉末压模压紧。例如,压模可为采用一模具和一个或多个模冲的单站式成型压机。或者,可采用仅使用一模具和单个下模冲的砧型压模。单站压模有几种基本类型,例如,具有不同生产能力的凸轮压力机、肘杆/肘板压力机和偏心/曲柄压力机,例如可以是单动、双动、浮动模压力机、可移动平板压力机、对置柱塞压力机、螺旋压力机、冲击式压力机、热压压力机、压印压力机或精整压力机。可以围绕阳极引线(如,钽线)压紧粉末。应当进一步理解的是,或者可以在阳极体压制和/或烧结后,将阳极引线固定(如,焊接)到阳极体上。
如果需要的话,可以在压制后,例如在某一温度(例如,从大约150℃到大约500℃)、真空条件下对成型颗粒加热几分钟,除去任何粘结剂/润滑剂。或者,也可将颗粒与水溶液接触而除去粘结剂/润滑剂,如Bishop等人的美国专利6,197,252所述,该专利以全文的形式通过引用引入本专利中用于所有目的。不管怎样,将压制的阳极体烧结以形成多孔的整块物质。烧结的条件可在上面提到的范围内。
然后,可将烧结的阳极体进行阳极氧化(“阳极化”),以在阳极上面和/或内部形成介电层。阳极氧化可以使用如上文所述的那些电解质溶液来进行。通常情况下,阳极发生阳极氧化的电压范围从大约4至大约250V,在一些实施方案中,从大约9到大约200V,以及在一些实施方案中,从大约20到150V。所得介电层可在阳极表面及其孔内形成。
所得阳极的尺寸部分取决于电容器要求的尺寸。在一些实施方案中,阳极体的长度是从大约1到大约100毫米,在一些实施方案中,阳极体的长度是从大约5到大约60毫米,以及在一些实施方案中,从大约5到大约20毫米。阳极的宽度(或直径)可从大约0.5到大约20毫米,在一些实施方案中,阳极的宽度从大约1到大约20毫米,以及在一些实施方案中,从大约4到大约10毫米。也可以选择阳极的形状,以改善所得电容器的电气性能。例如,阳极体可以是圆柱形、矩形、D-形和弧形等。
Ⅲ.工作电解质
工作电解质是一种可在阳极内浸渍的液体,或者它可以在生产后期加入到电容器内。液体电解质通常均匀地润湿阳极上的电介质。Evans等人的美国专利5,369,547和6,594,140中描述了多种合适的电解质。通常,电解质是离子电导的,其具有一电导率,在温度大约23℃,采用任何已知的电导仪(如Oakton Con Series11)测定的电导率从大约0.1到大约20西门子每厘米(“S/cm”),在一些实施方案中,从大约0.2到大约15S/cm,以及在一些实施方案中,从大约0.5到大约10S/cm。电解质通常是液体形式,例如溶液(例如水溶液或非水溶液)、胶状悬浮体、凝胶等。例如,电解质可以是酸的水溶液(如硫酸、磷酸或硝酸)、碱的水溶液(如氢氧化钾)、或盐的水溶液(例如铵盐,如硝酸盐)及本领域已知的任何其它合适的电解质,如溶解在有机溶剂中的盐(如溶解在乙二醇类溶液中的铵盐)。Evans等人的美国专利5,369,547和6,594,140中描述了多种其它电解质。
通过选择某一浓度范围的离子化合物(如酸、碱、盐等),可以实现要求的离子电导率。在一个具体的实施方案中,弱有机酸盐在实现要求的电解质电导率方面是有效的。盐的阳离子可以包括单原子阳离子,如碱金属(如Li+、Na+、K+、Rb+或Cs+)、碱土金属(如Be2+、Mg2+、Ca2+、Sr2+或Ba2+)、过渡金属(如Ag+、Fe2+、Fe3+等)以及多原子阳离子,如NH4+。一价铵(NH4+)、钠(K+)、锂(Li+)是尤其适合本发明的阳离子。用以形成盐的阴离子的有机酸可以是“弱”的,意思是指,在约23℃下测量,它通常具有约0至约11的第一酸离解常数(pKa1),在一些实施方案中为约1至约10,以及在一些实施方案中为大约2到大约10。任何合适的弱有机酸可用于本发明中,如羧酸,如丙烯酸、甲基丙烯酸、丙二酸、琥珀酸、水杨酸、磺基水杨酸、己二酸、马来酸、苹果酸、油酸、五倍子酸、酒石酸(例如右旋酒石酸(dextotartaric acid)、内消旋酒石酸等)、柠檬酸、甲酸、乙酸、乙醇酸、草酸、丙酸、邻苯二甲酸、间苯二甲酸、戊二酸、葡糖酸、乳酸、天冬氨酸、谷氨酸、衣康酸、三氟乙酸、巴比妥酸、肉桂酸、苯甲酸、4-羟基苯甲酸、氨基苯甲酸等;它们的共混物,等。在用于形成盐方面,多元酸(如二元酸、三元酸等)尤其符合要求,如己二酸(pKa1为4.43,pKa2为5.41)、α-酒石酸(pKa1为2.98和pKa2为4.34)、内消旋酒石酸(pKa1为3.22和pKa2为4.82)、草酸(pKa1为1.23和pKa2为4.19)、乳酸(pKa1为3.13,pKa2为4.76和pKa3为6.40)等。
实际用量可根据具体使用的盐、其在电解质所用溶剂中的溶解度和存在的其它组分而变化,此类弱有机酸盐通常以大约0.1到大约25wt.%的量存在于电解质中,在一些实施方案中,其量为大约0.2到大约20wt.%,在一些实施方案中,从大约0.3到大约15wt.%,以及在一些实施方案中,从大约0.5到大约5wt.%。
电解质通常是水溶液,因为它包含水相溶剂,如水(如去离子水)。例如,水(如去离子水)可占电解质的约20wt.%到约95wt.%,在一些实施方案中,占大约30wt.%到大约90wt.%,以及在一些实施方案中,占大约40wt.%到大约85wt.%。还可以使用第二溶剂,以形成溶剂混合物。合适的第二溶剂可以包括,例如,二醇(如乙二醇、丙二醇、丁二醇、三甘醇、己二醇、聚乙二醇、乙氧基二甘醇、二丙二醇等);乙二醇醚(如甲基乙二醇醚、乙基乙二醇醚、异丙基乙二醇醚等);醇(例如,甲醇、乙醇、正丙醇、异丙醇和丁醇);酮(例如,丙酮、甲基乙基酮和甲基异丁基酮);酯(例如,乙酸乙酯、醋酸丁酯、二乙二醇乙醚乙酸酯、丙二醇甲醚乙酸酯、碳酸乙二酯、碳酸丙二酯等);酰胺(例如,二甲基甲酰胺、二甲基乙酰胺、二甲基辛/癸脂肪酸酰胺和N-烷基吡咯烷酮);亚砜或砜(例如,二甲亚砜(DMSO)和环丁砜)等。此类溶剂混合物通常含从大约40wt.%到大约80wt.%的水,在一些实施方案中,含从大约50wt.%到大约75wt.%的水,以及在一些实施方案中,含从大约55wt.%到大约70wt.%的水,而第二溶剂的量为从大约20wt.%到大约60wt.%,在一些实施方案中,从大约25wt.%到大约50wt.%,以及在一些实施方案中,从大约30wt.%到大约45wt.%。例如,第二溶剂可占电解质的大约5wt.%到大约45wt.%,在一些实施方案中,占大约10wt.%到大约40wt.%,以及在一些实施方案中,占大约15wt.%到大约35wt.%。
如果需要的话,电解质可以相对中性,pH从大约4.5到大约8.0,在一些实施方案中,从大约5.0到大约7.5,以及在一些实施方案中,从大约5.5到大约7.0。为了帮助达到要求的pH值,可以使用一种或多种pH调节剂(如酸、碱等)。在一个实施方案中,采用酸将pH降低到要求范围。合适的酸包括,例如,上述各种有机酸;无机酸,如盐酸、硝酸、硫酸、磷酸、多磷酸、硼酸、有机硼酸(boronic acid)等;以及它们的混合物。虽然pH调节剂的总浓度可有所不同,但是,它们的量通常占电解质的大约0.01wt.%到大约10wt.%,在一些实施方案中,占大约0.05wt.%到大约5wt.%,以及在一些实施方案中,占大约0.1wt.%到大约2wt.%。
电解质还可以包含帮助改善电容器电气性能的其它组分。例如,在电解质中可以使用去极化剂,以帮助抑制电解电容器阴极处氢气的产生,氢气的产生会导致电容器膨胀,最终引发失效。使用去极化剂时,去极化剂在电解质中的含量通常从大约百万分之(“ppm”)1到大约百万分之500,在一些实施方案中,从大约10到大约200ppm,以及在一些实施方案中,从大约20到大约150ppm。合适的去极化剂可以包括硝基芳香化合物,如2-硝基苯酚、3-硝基苯酚、4-硝基苯酚、2-硝基苯甲酸、3-硝基苯甲酸、4-硝基苯甲酸、2-硝基苯乙酮、3-硝基苯乙酮、4-硝基苯乙酮、2-硝基茴香醚、3-硝基茴香醚、4-硝基茴香醚、2-硝基苯甲醛、3-硝基苯甲醛、4-硝基苯甲醛、2-硝基苄醇、3-硝基苄醇、4-硝基苄醇、2-硝基邻苯二甲酸、3-硝基邻苯二甲酸、4-硝基邻苯二甲酸等。尤其适合本发明使用的硝基芳香化合物去极化剂是被一个或多个烷基取代(如甲基、乙基、丙基、丁基等)的硝基苯甲酸及其酸酐或盐。此类烷基取代的硝基苯甲酸化合物的具体实例包括,例如,2-甲基-3-硝基苯甲酸;2-甲基-6-硝基苯甲酸;3-甲基-2-硝基苯甲酸;3-甲基-4-硝基苯甲酸;3-甲基-6-硝基苯甲酸;4-甲基-3-硝基苯甲酸;及它们的酸酐或盐等。
IV.密封组件
电容器的阳极和工作电解质通常置于外壳内部,所述外壳限定了一由密封组件封闭的开口。密封组件包括,例如,通常由绝缘材料如玻璃形成的密封件。如果需要,可采用孔的尺寸和形状足以容纳阳极引线的导电管。所述导电管一般由金属制成,例如钽、铌、铝、镍、铪、钛、铜、银、钢(如不锈钢)及它们的合金(如导电氧化物)、它们的复合物(如涂覆导电氧化物的金属)等。在这些实施方案中,导电管可通过密封件内的一穿孔,以使其电绝缘。
密封组件还可包括与至少部分密封件(如其下表面)接触的弹性隔障密封件。在一些实施方案中,弹性隔障密封可由一材料制成,该材料在较高温度下基本不降解或失去其机械性质,所述较高温度的范围如约150℃至约400℃,在一些实施方案中为约175℃至约350℃,以及在一些实施方案中为约200℃至约300℃(例如,200℃、225℃、250℃、275℃或300℃)。例如,这种高温弹性材料可展示出的“断裂伸长率”为约100%或以上,在一些实施方案中为约125%或以上,以及在一些实施方案中为约140%至约250%,和/或“断裂拉伸强度”为约2兆帕斯卡(“MPa”)或以上,在一些实施方案中为约5Mpa或以上,以及在一些实施方案中为约10Mpa至约25MPa,这些性质根据ASTM D412在拉伸夹头速度为500毫米每分钟下测量。注意,机械性质可在较宽的温度范围内得到保持,包括上述的高温,这能使密封件在极端条件下仍然发挥液体和/或蒸气屏障的作用。
虽然多种材料可以实现上面提到的性质,但是本发明者发现,全氟弹性体尤其有效,因为它们可以表现出所需的高温性能以及对工作电解质的高度耐腐蚀性。全氟弹性体的实例描述于,例如,Breazeale的美国专利4,281,092;Pittman等人的美国专利5,788,216;Park等人的美国专利7,718,736中。尤其适合用于本发明的全氟弹性体包括基本或全部由氟化单体单元衍生的交联共聚物,所述氟化单体单元如四氟乙烯和全氟(甲基乙烯基醚)单体单元。这些共聚物还可包含一额外的单体以辅助交联,如CF2=CF-O-CF2-CF(CF3)-O-C6F5、CH2=CH-CF2-CF2Br、CF2=CF-O-CF2CF(CF3)OCF2CF2CN和CF2=CH2。这些全氟弹性体可购自DuPont,商业名称为但其它合适的全氟弹性体可包括全氟甲基乙烯基醚和较高分子量的乙烯基醚的混合物与四氟乙烯的共聚物,该共聚物具有衍生自全氟烷基碘的硫化位点(cure site)单体。
密封件在电容器内的布置不是关键的,可按照本领域技术人员理解的方式改变。例如,参考图1,图中显示了电容器100的一个特定实施方案。如图所示,电容器100包含一外壳12,外壳12具有侧壁14和下壁16。在外壳不是圆柱形的这些实施方案中,可采用多个侧壁。如上所述,还在至少一部分外壳12上施加电化学活性材料17(例如,烧结的钽)。例如,电化学活性材料可设置在侧壁14和下壁16的内表面上。阳极20也置于外壳12的内部11中。阳极导线42可沿纵向穿过导电管56从阳极20伸出。
电容器100还包含密封组件50。在这个特定实施方案中,密封组件覆盖外壳12的卷折部分之间限定的开口59。或者,可提供如本领域所知限定开口的盖子。在任何情况下,在说明的实施方案中限定了一穿孔,导电管56和阳极引线42可穿过该穿孔,密封件54(例如,玻璃-金属密封)置于开口59内。密封组件50还包括一隔障密封件70,其由如上所述耐高温弹性材料形成。密封件70可具有基本为圆柱的形状并包含同轴置于其中的穿孔,导电管56和阳极引线42可穿过该穿孔。通过这种方式,隔障密封件70可覆盖密封件54的至少一部分下表面,以限制其与任何电解质的接触。如果需要,隔障密封件70可覆盖密封件54下表面的绝大部分。“绝大部分”通常指的是密封件覆盖约80%或以上的表面,在一些实施方案中覆盖大约90%或以上的表面,以及在一些实施方案中覆盖大约100%的表面。如图1所示,隔障密封件70一般还覆盖至少部分导电管56。
除上文所讨论的密封组件之外,本发明的电容器还可以包含一个或多个第二密封件。例如,可采用由非弹性绝缘材料如聚四氟乙烯(“PTFE”)制成的额外的垫圈或线轴(bobbin)。在一个实施方案中,例如,可将线轴90置于阳极20和隔障密封件70之间。例如也可采用邻近外壳12的侧壁14的弹性环92。弹性环92可由高温弹性体(例如上面描述的那些)或另一种类型的弹性材料制成。同样,如果需要,可提供与阳极接触的支撑体,以帮助确保其在使用过程中保持机械稳定性。支撑体可来自绝缘材料,例如聚四氟乙烯(“PTFE”)。这种支撑体的一个实例作为元件55显示在图2中,其邻接阳极20的下表面并与之接触。类似地,可通过焊接接头80将外部正极引线82连接到导电管56末端的阳极引线42,将外部负极引线83连接到外壳12的下壁16。
不管具体构造如何,本发明所得电容器都具有优异的电气性能。不管具体构造如何,本发明的电容器都具有优异的电气性能。例如,电容器具有较高的体积效率,例如,在频率120Hz及室温(如25℃)时测定的体积效率从大约50,000μF*V/cm3至大约300,000μF*V/cm3,在一些实施方案中,从大约60,000μF*V/cm3到大约200,000μF*V/cm3,以及在一些实施方案中,从大约80,000μF*V/cm3至大约150,000μF*V/cm3。将部件的形成电压乘以其电容,然后将所得乘积除以部件体积即得到体积效率。例如,部件的电容520μF,形成电压是175伏特,两者的乘积是91,000μF*V。如果部件占据的体积是大约0.8cm3,则体积效率大约是113,750μF*V/cm3。
电容器还具有高能量密度,使其适合高脉冲应用。能量密度通常按照公式E=1/2*CV2确定,其中C是以法拉(F)表示的电容,V是以伏特(V)表示的电容器工作电压。电容器可以例如使用电容表(例如,Keithley3330Precision LCZ电容表,带有Kelvin引线,2伏特偏压,1伏特信号)在10-120Hz(例如120Hz)的工作频率和25℃下测定。例如,电容器显示出的能量密度为约2.0焦耳每立方厘米(J/cm3)或以上,在一些实施方案中为约3.0J/cm3,在一些实施方案中为约3.5J/cm3至约10.0J/cm3,以及在一些实施方案中为约4.0J/cm3至约8.0J/cm3。类似地,电容为大约1毫法拉每平方厘米(“mF/cm2”)或更高,在一些实施方案中,为约2mF/cm2或更高,在一些实施方案中,从大约5到大约50mF/cm2,以及在一些实施方案中,从大约8到大约20mF/cm2。电容器也可具有相对较高的“击穿电压”(电容器失效时的电压),如大约180V或更高,在一些实施方案中,大约200V或更高,以及在一些实施方案中,从大约210V到大约260V。此外,漏电流通常指的是从一个导体通过绝缘体流向邻近导体的电流,它可以维持在相对较低的水平。例如,本发明电容器的归一化漏电流的数值,在一些实施方案中低于大约1μA/μF*V,在一些实施方案中,低于大约0.5μA/μF*V,以及在一些实施方案中,低于约0.1μA/μF*V,其中μA是微安,μF*V是电容和额定电压的乘积。漏电流可在温度25℃以及在某一额定电压下在充电大约60秒到大约300秒后,使用漏电测试仪(例如,MC190漏电测试仪,Mantracourt Electronics LTD,UK)来测定。这样的归一化漏电流值甚至可在高温(如上面所描述的)下维持很长的时间。
本发明的电解电容器可用于各种应用,包括但不限于微型逆变器;微型UPS设备;医疗设备,如植入式除纤颤器、起搏器、心电复律器、神经刺激器、给药装置等;汽车应用;军事应用,如雷达系统;消费者电子产品,如收音机、电视等。例如,在一个实施方案中,电容器可用于植入式医疗设备中,为患者提供高电压治疗(如约500伏特至约850伏特之间,或者,如果需要的话,大约600伏特到约900伏特之间)。该设备可包含一密封并具生物惰性的容器或外壳。一个或多个导联通过血管在设备与患者心脏之间电耦合。心脏电极的配备用以感应心搏和/或向心脏提供电压。至少一部分导联(例如,导联的末端部分)可设置于心脏的一个或多个心室和心房附近或与其接触。该设备还包含一个电容器组,所述电容器组一般包含两个或多个串联连接的电容器,并与设备内部或外部的电池连接,为电容器组提供能量。部分是由于电导率较高,本发明的电容器具有优异的电气性能,因此,适合用于植入式医疗设备的电容器组。
通过下述实施例可以更好地理解本发明。
实施例1
如本文所描述组装86μF/100V的样品,其带有经阳极氧化的钽阳极、阴极和硫酸工作电解质,所述阴极包含圆柱形钽罐内表面上的烧结的钽涂层。在施加烧结的钽涂层前,将钽罐的内表面在5、7和10V的形成电压下进行阳极化。所得电容器在200℃下施加60和75V电压测试ESR。结果见图2。如图所示,5Vf阴极的ESR在600小时后获得了117%的增加,而7Vf阴极仅获得23%的增加,10Vf阴极只获得2.4%的增加。在75V的过量电压条件下测定的电容器在600小时后ESR获得了262%的增加,而7Vf阴极的电容器ESR获得197%的增加,以及10Vf阴极的电容器ESR获得100%的增加.
实施例2
如本文所描述组装120μF/100V的样品,其带有经阳极氧化的钽阳极、阴极和硫酸工作电解质,所述阴极包含圆柱形钽罐内表面上的烧结的钽涂层。样品中包含如本文描述的弹性隔障密封件。所得电容器在200℃下施加60V电压测定ESR。结果见图3。如图所示,电容器在600小时以后仅获得了27%的增加。
在不偏离本发明的实质和范围下,本领域技术人员可实施本发明的这些和其它的改良和变形。另外,应该理解,各个实施方案的各方面可整体或部分相互替换。并且,本领域技术人员应该明白,上文仅以实施例的方式对本发明进行说明,并不用于对本发明进行限制,将在权利要求书中对本发明做进一步说明。
Claims (26)
1.一种湿式电解电容器,包括:
一外壳,其限定一开口和包围内部的侧壁,其中该外壳包含一用电化学活性材料涂覆的金属基体;
一阳极,其置于所述外壳内部,其中所述阳极由经阳极氧化的烧结的多孔主体形成,所述阳极包含从中伸出的阳极引线;以及
液体工作电解质,其与阳极及电化学活性材料电接触;
其中,用2伏特偏压和1伏特信号在120Hz的频率下测量,该湿式电解电容器在200℃的温度下表现出约3000毫欧姆或以下的等效串联电阻。
2.根据权利要求1所述的湿式电解电容器,其中介电层存在于金属基体上,其厚度为约10纳米至约500纳米。
3.根据权利要求2所述的湿式电解电容器,其中所述介电层的厚度为约20至约100纳米。
4.根据前述权利要求要求任一项所述的湿式电解电容器,进一步包括覆盖所述开口的密封组件,该密封组件包括一密封件和一隔障密封件,其中所述隔障密封件包含弹性材料。
5.根据权利要求4所述的湿式电解电容器,其中所述弹性材料包括全氟弹性体。
6.根据权利要求4或5所述的湿式电解电容器,其中按照ASTM D412进行测定,在500毫米每分钟的拉伸夹头速度,在200℃的温度下,所述弹性材料展示出在断裂时约100%或以上的伸长率和/或断裂时约2兆帕斯卡或以上的拉伸强度。
7.一种湿式电解电容器,包括:
一外壳,其限定了一开口和包围内部的侧壁,其中所述外壳包含一阳极氧化的金属基体,该基体具有厚度为约10纳米至约500纳米的介电层,其中所述金属基体涂覆有电化学活性材料;
一阳极,其置于所述外壳内部,其中所述阳极由经阳极氧化的烧结的多孔主体形成,所述阳极包含从中伸出的阳极引线;以及
液体工作电解质,其与阳极及电化学活性材料电接触。
8.一种湿式电解电容器,包括:
一外壳,其限定一开口和围绕内部的侧壁,其中该外壳包含一用电化学活性材料涂覆的金属基体;
一阳极,其置于所述外壳内部,其中所述阳极由经阳极氧化的烧结的多孔主体形成,所述阳极包含从中伸出的阳极引线;
液体工作电解质,其与阳极及电化学活性材料电接触;以及
一密封组件,其覆盖所述外壳的开口,并包含密封件和隔障密封件,其中所述隔障密封件包含一弹性材料,按照ASTM D412进行测定,在500毫米每分钟的拉伸夹头速度,在200℃的温度下,所述弹性材料展示出在断裂时约100%或以上的伸长率和/或断裂时约2兆帕斯卡或以上的拉伸强度。
9.根据权利要求8所述的湿式电解电容器,其中所述弹性材料包括全氟弹性体。
10.根据前述权利要求任一项所述的湿式电解电容器,其中所述金属基体由钽形成。
11.根据前述权利要求任一项所述的湿式电解电容器,其中所述金属基体形成整个或部分外壳。
12.根据前述权利要求任一项所述的湿式电解电容器,其中所述电化学活性材料包括烧结的钽颗粒。
13.根据前述权利要求任一项所述的湿式电解电容器,其中所述电化学活性材料包括导电聚合物。
14.根据前述权利要求中任一项所述的湿式电解电容器,其中,所述阳极包含钽。
15.根据前述权利要求中任一项所述的湿式电解电容器,其中,所述工作电解质是液体。
16.根据权利要求1-15中任一项所述的湿式电解电容器,其中所述工作电解质是含硫酸的水溶液。
17.根据权利要求1-15中任一项所述的湿式电解电容器,其中所述工作电解质的pH值为约4.5至约8.0。
18.根据前述权利要求中任一项所述的湿式电解电容器,进一步包含一延伸穿过密封件和/或隔障密封件的导电管,其中所述阳极引线延伸穿过所述导电管。
19.根据权利要求18所述的湿式电解电容器,进一步包含一密封在所述导电管末端的外部正极引线和密封至所述外壳下壁的外部负极引线。
20.根据前述权利要求中任一项所述的湿式电解电容器,其中,所述隔障密封件与所述密封件接触。
21.根据权利要求19所述的湿式电解电容器,其中所述隔障密封件覆盖所述密封件表面的绝大部分。
22.根据前述权利要求中任一项所述的湿式电解电容器,进一步包含一线轴,其邻近所述阳极的上表面,所述线轴由绝缘材料形成。
23.根据前述权利要求中任一项所述的湿式电解电容器,进一步包含邻近所述外壳侧壁放置的弹性环。
24.一种形成电解电容器的方法,该方法包括:
通过阳极氧化一金属基体,以在其上形成厚度约10纳米至约500纳米的介电层,然后用电化学活性材料涂覆基体,形成一外壳;
将阳极放置在所述外壳的内部,其中所述阳极由阳极氧化的烧结的多孔主体形成,所述阳极包含一从中伸出的阳极引线;以及
放置液体工作电解质,使其与所述阳极和电化学活性材料电接触。
25.根据权利要求24所述的方法,其中通过将所述基体放在电解质槽中并通入电流使所述金属基体阳极氧化。
26.根据权利要求25所述的方法,其中所述电流在约7伏特或以上的形成电压下施加。
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US20140268498A1 (en) | 2014-09-18 |
CN104051159B (zh) | 2018-06-12 |
GB2512481A (en) | 2014-10-01 |
US9384901B2 (en) | 2016-07-05 |
GB201403080D0 (en) | 2014-04-09 |
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GB2512481B (en) | 2018-05-30 |
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