CN101673620A - 用于湿化电容的基底 - Google Patents
用于湿化电容的基底 Download PDFInfo
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- CN101673620A CN101673620A CN200910164879A CN200910164879A CN101673620A CN 101673620 A CN101673620 A CN 101673620A CN 200910164879 A CN200910164879 A CN 200910164879A CN 200910164879 A CN200910164879 A CN 200910164879A CN 101673620 A CN101673620 A CN 101673620A
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- negative electrode
- wet capacitors
- acid
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Abstract
本发明涉及多孔基底,具备广泛的应用,如湿化电容。所述基底通过将金属基底在溶液中加电压以阳极化产生氧化物膜的方法制备。与传统的阳极化过程相反,新生成的氧化物迅速分解以再次使金属表面暴露于电解质溶液。可以通过多种方法实现,如通过将溶液的电压提高至高于临界值即“分解电压”;或者采用溶液中的腐蚀性酸以溶解氧化物;等等。无论以何种原理,几乎同步的氧化物生长/分解过程能够形成具有规律间隔的孔的结构。得到的结构为高度多孔的,对电化学活性材料能良好附着,在水性电解液中稳定。
Description
技术领域
本发明涉及用于湿化电容的阴极结构及其制备方法。
背景技术
湿化电容由于其容积效率、可靠性以及工艺兼容性,被越来越广泛地应用于电路设计中。湿化电容典型的比其他类型的电容具有更高的单位体积电容,从而在高电流、高功率和低频电路中显得更加难得。开发的湿化电容的一种类型为包括阀金属阳极、阴极和液体电解质的湿化电解电容。由于在阳极表面形成金属氧化物介质膜,这类电容的单位体积电压(unit cellvoltage)普遍较高。湿化电解电容往往提供高电容、低泄漏电流的良好组合。另一种湿化电容为湿化对称电容,其中,阳极和阴极的结构和组成类似。该类型电容的单位体积电压普遍较低,是由于电解质在高电压下难免产生的分解。无论是电解型还是对称型,湿化电容的阴极通常包括基底和涂层,所述涂层通过法拉第模式或者非法拉第模式提供高电容。为了提高这些涂层的附着性,基底有时被机械性和/或化学性刻蚀。然而在某些条件下,例如在水性电解液存在下,涂层依然容易与基底脱离。
因此,目前需要一种用于湿化电容中的改进的阴极。
发明内容
本发明的一个实施方式,公开了一种湿化电容,包括阳极、阴极以及位于阴极和阳极间的工作电解液。所述阴极具有阳极化的金属基底,被电化学活性的材料涂敷。该基底包含多个形成于表面的孔,该孔的平均尺寸为约10-约1500纳米。
另一个实施方式公开了一种电气导电阴极,其具有阳极化的金属基底,被导电聚合物涂敷,其中所述基底包含多个形成于表面的孔,该孔的平均尺寸为约20-约1000纳米。
进一步,另一个实施方式公开了形成用于湿化电容的阴极的方法。所述方法包括将金属基底浸渍在阳极化溶液中;在金属基底上应用第一电压下的电流以影响阳极氧化并形成包含氧化物膜的阳极化的基底;启动分解氧化物膜以在阳极化基底的表面上形成多个孔,所述孔的平均尺寸为约10-约1500纳米。
本发明的其他方面特征在以下内容中详述。
附图说明
在以下内容中完整详细的公开本发明,包括其最优的实施方式,并结合附图说明:
图1为根据本发明电容的一个实施例的横截面图;
图2为用于实施例1中的电压曲线图;
图3为实施例1中形成的基底的SEM照片(20kV,10000×);
图4为实施例2中形成的基底的SEM照片(25kV,10000×);
图5为实施例3中形成的基底的SEM照片(25kV,10000×);
图6为实施例4中形成的基底的SEM照片(15kV,10000×);
图7为实施例5中形成的基底的SEM照片(20kV,10000×);
图8为实施例6中形成的基底的SEM照片(15kV,10000×);
图9为用于实施例8中电压的曲线图。
附图中相同的附图标记表示本发明中相同或相似的特征或元件。
具体实施方式
本领域的技术人员应该理解,这里讨论的实施例只是示例性质,不应用来限制本发明的范围,本发明更广的范围建立在实施例的基础上。
通常,本发明的基底广泛用于各种应用中,例如湿化电容。基底通过在金属基底上加压同时在溶液中启动阳极化形成氧化物膜形成。与传统的阳极化不同,新产生的氧化物迅速分解从而再次将金属表面暴露于电解质溶液中。可以通过不同方法实现,例如将溶液电压提高到一个称为“分解电压”的临界值以上,然后采用腐蚀性酸溶解氧化物,等。不考虑使用的原理,几乎同步的氧化物生长/分解过程导致具有规则间隔的孔结构的形成。所述得到的结构高度有序并且为多孔的,可以表现出对电化学活性材料的高附着性以及在水性电解液中的稳定性。
金属基底可以包括任何金属,例如钽、铌、铝、镍、铪、钛、铜、银、钢(如不锈钢),以及它们的合金,等。为本领域技术人员所熟知的,基底的几何结构通常可以变化,例如为容器状、听状、箔状、片状、筛状等。
可以采用任何技术将基底与阳极化溶液接触,例如浸蘸、喷洒、涂敷等。然而,阳极化溶液通常包含一种或多种离子化合物(即含有一种或多种离子的化合物或在溶液中能够形成一种或多种离子的化合物)以启动阳极氧化。合适的离子化合物可以包括无机酸,如硝酸、磷酸、多磷酸(polyphosphoric acid)、硼酸、烃基硼酸(boronic acid)等;有机酸,包括羧酸,例如丙烯酸、甲基丙烯酸、丙二酸、丁二酸、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、蚁酸、乙酸、羟基乙酸、草酸、丙酸、邻苯二甲酸、间苯二甲酸、戊二酸、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,例如甲基磺酸、苯磺酸、甲苯磺酸、三氟甲磺酸、苯乙烯磺酸、萘二磺酸、羟基苯磺酸等;聚合物酸,例如聚(丙烯酸)或聚(甲基丙酸烯)以及它们的共聚物(例如马来酸-丙烯酸共聚物、磺酸-丙烯酸共聚物以及苯乙烯-丙烯酸共聚物),角叉菜酸(carageenic acid),羧甲基纤维素、褐藻酸等等。溶液的离子电导率通常为约50mS/cm或更高,在一些实施例中为约100mS/cm或更高,在另一些实施例中为约125-约1000mS/cm。
可以在溶液中施加某一电压(如正电压)下的电流(如直流电),该电压低于临界的“分解”电压值(氧化物“形成”阶段),从而使得氧化物能够以大致线性速率开始生长。这一阶段实际应用的电压可能基于基底的本性、溶液的本性、所需绝缘膜厚度以及电流密度而不同,但是通常在约1V-约140V的范围内,在一些实施例中为在约5V-约130V之间,在一些实施例中为在约10V-约120V之间。电压可能在这一范围内变化(如上升)或保持不变。
如上所述,本发明可以采用不同的模式使得形成的氧化物分解以形成孔。例如在一个实施例中,在“形成”阶段之后电压上升到临界电压(“分解”阶段)之上以启动如上所述的交替的氧化物形成和分解过程。这一过程可能在恒定电流或在脉冲电压下进行。临界分解电压通常在约45V-约200V之间,在一些实施例中为在约50V-约140V之间,在一些实施例中为在约55V-130V之间。在“分解”阶段,电压可能变化(如上升)或保持不变。例如在一个实施例中,电压在“分解”阶段上升,从而使得氧化物膜的部分或完全恢复拥有足够的时间。这一上升可能为不超过现有电压的50%,在一些实施例中为不超过25%,在一些实施例中为不超过10%。例如,上升可能为不超过现有电压约30V,在一些实施例中为不超过约15V,在一些实施例中为不超过5V。
不仅仅是简单的提高电压,还应该理解的是,逆向脉冲电压技术(reversepulse voltage techniques)也可以用于启动交替的氧化物膜形成和分解过程。例如,最初在氧化物形成阶段采用正电压,在分解阶段采用负电压,该负电压改变氧化物的极性从而导致分解。
也可以采用化合物启动氧化物膜的分解。例如在一个实施例中,可以采用腐蚀性酸或盐在氧化物膜形成中分解氧化物膜。这类腐蚀性化合物的例子为氯化氢、硫酸、氟化铵、氟化钠、氟化钾等。采用时,理想地可控制腐蚀性酸在阳极化溶液中的含量从而使得氧化物膜不会大范围分解。在这一方面,在阳极化溶液中采用的离子化合物相对于腐蚀性酸的质量比通常为约5∶1-约50∶1,在一些实施例中为约10∶1-约40∶1,在一些实施例中为约12∶1-约25∶1。
可以控制其他参数以达到基底中所需的孔隙率。在形成和/或分解阶段中阳极化溶液的温度可以为接近室温,例如约10℃-约50℃,在一些实施例中为约15℃-约40℃,在一些实施例中为约20℃-约30℃。电流密度典型的为约0.005-约0.5A/cm2,在一些实施例中为约0.08-约0.30A/cm2,在一些实施例中为约0.01-约0.1A/cm2。温度和电流密度可能在形成和/或分解阶段变化或保持不变。
如果需要,多孔基底也可以进行加热步骤使得金属基底的氧化最小化。基底加热的温度依赖于用于阳极体中的组成类型。例如,基底通常在炉内加热,操作温度为约200℃-约1400℃,在一些实施例中为约300℃-约1200℃,在一些实施例中为约400℃-约1000℃。加热可以为约5-300分钟,在一些事实力中为约10-约200分钟,在一些实施例中为约15-约90分钟。加热通常在还原气氛(reducing atmosphere)下进行,如真空、惰性气体、氢气等等。如果需要,也可以采用吸气材料,该吸气材料能够与加热处理中排出的氧原子结合,进一步提高电导率,例如钽、铌、碳、镁等,或者它们的组合。
如上所述的过程的结果是,形成的金属基底为高度多孔的。孔径足够小使得能够有效的增加基底的表面积,又足够大使得电化学活性材料能够从中通过。在这一方面,孔径平均尺寸通常为约10-约1500纳米,在一些实施例中为约20-约1000纳米,在一些实施例中为约50-约500纳米。孔的形状可以是圆形、管状、方形、长方形等。这些管状的孔的深度可以为约10-约800纳米,在一些实施例中为约20-约600纳米,在一些实施例中为约30-约400纳米。除了孔的尺寸和形状,还可以控制孔隙率。例如,孔可能占基底表面的约10%-约90%,在一些实施例中为约20%-约80%,在一些实施例中为约30%-约70%。
另外,分解过程后任何残留在基底表面的氧化物膜非常薄,不会在表面形成连续的涂层。也就是,表面被金属和被氧化物涂敷的金属区域定义。因此,多孔基底可以保持高电导率。电导率可以用约20℃的“电阻系数”表示,通常为低于约1ohm-cm,在一些实施例中为低于约1×10-2ohm-cm,在一些实施例中为低于约1×10-3ohm-cm,在一些实施例中为低于约1×10-4ohm-cm。虽然是导电的,基底仍可能被额外层涂敷一种导电材料从而进一步提高表面的导电性。这类材料的例子可以包括金属,例如金、铂、钯、铜、银等。
一旦形成,电化学活性材料应用于多孔基底上以增加有效表面积,在该表面上电解液与基底电化学连接(communicate)。这一增加的有效表面积能够形成特定尺寸的具有提高的阴极电容的电容器和/或形成特定电容的具有更小尺寸的电容。通常可以采用任何已知的电化学活性材料。例如在一个实施例中,可以采用导电聚合物,例如聚吡咯;聚噻吩,例如聚(3,4-乙烯基二氧噻吩)(PEDT);聚苯胺;聚乙炔;聚对苯撑;它们的衍生物等。如本领域所熟知的,这些导电聚合物可以由单体聚合形成无定形的非晶态,在扫描电子显微镜下看上去形态像是网。也就是,得到的导电聚合物涂层具有较高的表面积,因此能够增加其应用的基底的有效表面积。
导电聚合物涂层可能包括一个或多个导电聚合物层,可以使用不同的已知方法得到。例如,可以采用筛印(screen-printing)、浸渍、电泳涂敷以及喷洒以形成涂层。例如在一个实施例中,用于形成导电聚合物(如PEDT)的单体可以最初与聚合催化剂混合以形成分散系。一种合适的聚合催化剂为CLEVIOS C(Bayer Corp.),其为Fe(III)甲苯-磺酸盐及n-丁醇。CLEVIOS C为CLEVIOUS M的商用催化剂,CLEVIOUS M为3,4-乙烯基二氧噻吩,它是一种由Bayer公司销售的PEDT单体。一旦分散系形成,可以将基底浸渍于分散系中从而形成导电聚合物。或者,可以分别应用催化剂和单体。例如,催化剂可以溶于溶剂(如丁醇),接着作为浸渍溶液应用,虽然以上叙述了各种不同的方法,应该理解的是,可以使用任何其他应用含有导电聚合物涂层的涂层的方法。例如,其他应用含有一种或多种导电聚合物的涂层的方法记载在Sakata等人的美国专利5457862、5473503、5729428和Kudoh等人的美国专利5812367中,在此以全文引用的方式引用作为参考。
除了导电聚合物,还可以采用金属,如由钌、铱、镍、铑、铼、钴、钨、锰、钽、铌、钼、铅、钛、铂、钯和锇形成的金属颗粒,以及这些金属的组合。例如在一个特别的实施例中,电化学活性材料包括钯颗粒。本发明还可以采用非绝缘氧化物颗粒。合适的氧化物可以包括选自钌、铱、镍、铑、铼、钴、钨、锰、钽、铌、钼、铅、钛、铂、钯和锇,以及它们的组合的金属。特别合适的金属氧化物包括二氧化钌、氧化铌、二氧化铌、氧化铱以及二氧化锰。也可以采用具有理想电导率的含碳颗粒,例如活性炭、炭黑、石墨等。一些合适的活性炭形式和形成技术在Ivey等人的美国专利5726118,Wellen等人的美国专利5858911以及Shinozaki等人的美国专利申请2003/0158342中有记载,在此以全文引用的方式引用作为参考。
如果需要,可以采用粘合剂以辅助将电化学活性材料粘合于基底上。任何提供所需粘合强度的粘合剂都可以使用。例如,合适的粘合剂可以包括聚四氟乙烯、聚偏二氟乙烯、羧甲基纤维素、氟烯烃共聚物交联聚合物(fluoroolefin copolymer crosslinked polymer)、聚乙烯醇、聚丙烯酸、聚酰亚胺、石油沥青、煤沥青、以及苯酚树脂。在一些实施例中还可以采用导电填料以进一步提高电化学活性材料的电导率。这类导电填料可以特别有效的抵消由于粘合剂覆盖电化学活性材料的部分表面导致的电导率下降。可以采用任何合适的导电填料,例如金属颗粒(如银、铜、镍、铝等);非金属颗粒(如炭黑、石墨等)。
本发明的结果是,可以形成具有相对较高比电容的电极。例如,电极的比电容在频率为120Hz的5.0M硫酸溶液中测定,可以为约10mF/cm2或更高,在一些实施例中为约15mF/cm2或更高,在一些实施例中为约25-约100mF/cm2。高的电容值甚至可以在相对较低的总厚度下得到,该厚度为约100微米或更低,在一些实施例中为约75微米或更低,在一些实施例中为约10-约50微米。如此薄而高电容的电极适用于许多应用,包括对称和非对称湿化电容、电池等。例如在一个实施例中,可以在一个非对称的湿化电解电容中采用阴极,所述电容包括阳极、阴极以及一个位于二者之间且与阳极和阴极接触的工作电解液。在这方面,这类湿化电解电容的不同实施例可以根据本发明形成,在此将详述。应该理解的是,下述记载只是示例性质,本发明也能形成多种其他的实施例。
湿化电解电容的阳极通常由多种不同材料形成。例如,阳极可以由粉末形成,粉末主要由阀金属(能够氧化的金属)或含有阀金属作为组分的组合物形成。可以使用的合适的阀金属包括而不限于:钽、铌、铝、铪、钛以及它们的合金等。例如,阳极可以由阀金属氧化物或氮化物(如:氧化铌、氧化钽、氮化钽、氮化铌等)形成,这些阀金属氧化物或氮化物通常被认为是半导体或高电导率的材料。特别适合用作阳极的阀金属氧化物包括氧化铌,其铌原子相对于氧原子比为1∶2.5或更大,在一些实施例中为1∶1.5或更大,在一些实施例中为1∶1.1或更大,在一些实施例中为1∶1.0±0.2。例如,氧化铌可以为Nb0.7、NbO1.0、NbO1.1以及NbO2。这类阀金属氧化物的其他例子在Fife的美国专利6322912中有记载,在此以全文引用的方式引用作为参考。这类阀金属氮化物的例子在2000年3月6日-20日举行的“Proceedings of CARTS 2000:20th Capactor and Resistor TechnologySymposium”中T.Tripp的“Tantalum Nitride:A New Substrate for SolidElectrolytic Capacitors”中有记载。
通常可以使用不同的传统的制造方法制造阳极。例如,如在本领域熟知的,阳极可以形成为箔、粉末压片等。示例性的粉末压片记载在Fife等人的美国专利7099143中,在此以全文引用的方式引用作为参考。或者,阳极可以由陶瓷颗粒(如Nb2O5、Ta2O5)形成,这些陶瓷颗粒化学还原形成电气导电材料(如NbO、Ta)。例如,可以先形成含有陶瓷颗粒的粉浆混和物(slip composition)并以薄层形式沉积于基底。如果需要,可以形成多层得到阳极的目标厚度。一旦形成,层加热以化学还原陶瓷颗粒并形成电气导电的阳极。这类滑模形成的(slip-formed)阳极可以具有低厚度,高横纵比(宽度比厚度)以及均匀的密度,从而改进容积效率和等效串联电阻(ESR)。例如,阳极的厚度可以为约1500微米或更低,在一些实施例中为约1000微米或更低,在一些实施例中为约50-约500微米。同样的,阳极的横纵比为约1或更高,在一些实施例中为约5或更高,在一些实施例中为约15或更高。
阳极可以具有理想的形状,如正方形、长方形、圆形、椭圆形、三角形等。具有超过4边的多边形(如六边形、八边形、七边形、五边形等)是特别理想的,是因为它们相对更高的表面积。阳极也可以具有“凹槽”形状,具有一个或多个皱纹、凹槽、凹陷或锯齿以增加表面积和体积比,从而使ESR最小化,并扩展电容的频率响应。这些“凹槽”形阳极记载在Webber等人的美国专利6191936、Maeda等人的美国专利5949639、Bourgault等人的美国专利3345545以及Hahn等人的美国专利申请2005/0270725中,在此以全文引用的形式引用作为参考。
一旦形成,阳极可以阳极化使得在阳极上和内形成绝缘膜。例如,氧化铌(NbO)阳极可以阳极化形成五氧化二铌(Nb2O5)。特别的,在一个实施例中,氧化铌阳极在高温下(如85℃)浸渍在弱酸溶液中(如磷酸、多磷酸、它们的混合物等),同时施以可控的电压和电流,从而形成具有一定厚度的五氧化二铌涂层。最初的电源为稳定电流,直到达到所需的形成电压。此后,电源保持为稳定电压,以保证所需的绝缘厚度在阳极表面形成。阳极化电压通常为约10-约200V,在一些实施例中为约20-约100V。除了在阳极表面形成,部分绝缘氧化膜也通常在材料的孔表面形成。应该理解的是,绝缘膜可以由其他类型的材料形成,以及使用不同技术形成。
工作电解液为电活性材料,提供在阳极和阴极间的连接路径,通常为液体形式,例如溶液(如水性或非水性),分散系、凝胶体等。例如,工作电解液可以为酸的水性溶液(如硫酸、磷酸、或硝酸),碱(如氢氧化钾)或者盐(如铵盐,例如硝酸盐)以及本领域任何合适的工作电解液,例如溶于有机溶剂的盐(如溶于乙二醇的铵盐溶液)。其他不同的电解液记载在Evans等人的美国专利5369547、6594140中,在此以全文引用的形式引用作为参考。
在一个特别的实施例中,电解液为相对中性的,pH为约3.0-约8.0,在一些实施例中为约4.0-约7.5,在一些实施例中为约5.0-约7.5。尽管具有中性的pH值,该电解液为电气导电的。例如,该电解液的电导率在25℃测定为约10mS/cm或更高,在一些实施例中为约30mS/cm或更高,在一些实施例中为约40mS/cm-约100mS/cm。电导率的值可以用已知的电导仪(如Oakton ConSeries 11)在25℃测定。
工作电解液可以包括不同的组分以优化其电导率、pH、以及在电容储存和使用中的稳定性。例如,通常采用溶剂作为电解液其余组分的载体。该溶剂可以由电解液的约30wt.%-约90wt.%组成,在一些实施例中为约40wt.%-约80wt.%,在一些实施例中为约45wt.%-约70wt.%。可以采用任何溶剂,例如水(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、丁醇);甘油三酸酯;酮(如丙酮、甲基乙基酮、甲基异丁基酮);酯(如乙酸乙酯、丁基乙酯、二乙烯基乙二醇醚乙酯、甲氧基丙基乙酯);酰胺(如二甲基甲酰胺、二甲基乙酰胺、二甲基辛酸/癸酸脂肪酸酰胺和N-烷基吡咯烷酮);腈(如乙腈、丙腈、丁腈、氰苯);亚砜或砜(如二甲基亚砜(DMSO)和环丁砜);等等。虽然不是必须的,通常理想的使用水性溶剂(如水)以辅助保持电解液的pH在相对中性水平。实际上,水可以组成电解液中使用的溶剂的约50wt.%或更多,在一些实施例中为约70wt.%或更多,在一些实施例中为约90wt.%-100wt.%。
工作电解液的电导率可以通过一种或多种离子化合物提供,如上述所述的离子化合物。选择离子化合物的浓度以达到电导率和pH之间理想的平衡。也就是,可以采用强酸(如磷酸)作为离子化合物,虽然通常限制它的浓度以保持在理想的pH水平。强酸通常组成电解液的约0.001wt.%-约5wt.%,在一些实施例中,为约0.01wt.%-约2wt.%,在一些实施例中,为约0.1wt.%-约1wt.%。另一方面,可以采用弱酸(如乙酸),只要能够达到所需的电导率。弱酸通常组成电解液的约1wt.%-约40wt.%,在一些实施例中为约2wt.%-约30wt.%,在一些实施例中为约5wt.%-约25wt.%。如果需要,可以采用在电解液中混合弱酸和强酸。离子化合物的总浓度可能不同,但通常为电解液的约1wt.%-约50wt.%,在一些实施例中为约2wt.%-约40wt.%,在一些实施例中为约5wt.%-约30wt.%。
如果需要,可以在电解液中采用碱性pH调节剂,其量能够有效的平衡离子化合物对pH的影响。合适的碱性pH调节剂可以包括但不限于:氨;单、二和三烷基胺;单、二和三链烷醇胺;碱金属和碱土金属氢氧化物;碱金属和碱土金属硅酸盐;以及它们的混合物。碱性pH调节剂的例子为氨;氢氧化钠、钾、锂;偏硅酸钠、钾、锂;单乙醇胺;三乙胺;异丙胺;二乙醇胺;以及三乙醇胺。
为了保证电解液在正常储存条件下的稳定,通常理想的,其凝固点为约-20℃或更低,在一些实施例中为约-25℃或更低。如果需要,可以采用一个或多个凝固点抑制剂,如二醇(如丙二醇、丁二醇、三乙二醇、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);等等。虽然凝固点抑制剂的浓度不同,通常在电解液中为约5wt.%-约50wt.%,在一些实施例中为约10wt.%-约40wt.%,在一些实施例中为约20wt.%-约30wt.%。还应注意的是,电解液的沸点通常为约85℃或更高,在一些实施例中为约100℃或更高,使得电解液在高温下保持稳定。
在工作电解液中还可以采用退极化剂以辅助抑制在电解电容器阴极产生氢气,否则会导致电容膨胀并最终失效。退极化剂通常在电解液中为约1-约500ppm,在一些实施例中为约10-约200ppm,在一些实施例中为约20-约150ppm。
合适的退极化剂可以包括芳硝基化合物,如2-硝基苯酚、3-硝基苯酚、4-硝基苯酚、2-硝基苯甲酸(2-nitrobenzonic acid)、3-硝基苯甲酸(3-nitrobenzonic acid)、4-硝基苯甲酸(4-nitrobenzonic acid)、2-硝基苯乙酮(2-nitroacetophenone)、3-硝基苯乙酮(3-nitroacetophenone)、4-硝基苯乙酮(4-nitroacetophenone)、2-硝基苯甲醚、3-硝基苯甲醚、4-硝基苯甲醚、2-硝基苯甲醛、3-硝基苯甲醛、4-硝基苯甲醛、2-硝基苯甲醇、3-硝基苯甲醇、4-硝基苯甲醇、2-硝基邻苯二甲酸、3-硝基邻苯二甲酸、4-硝基邻苯二甲酸、等等。特别适用于本发明的芳硝基退极化剂为硝基苯甲酸、它们的酸酐或盐,具有一个或多个烷基(如甲基、乙基、丙基、丁基等等)。这里烷基取代的硝基苯甲化合物包括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-苯甲酸;4-甲基-3-硝基苯甲酸,它们的酸酐或盐等等。不限于理论,相信当阴极电势达到较低区域或槽电压(cell voltage)较高时,烷基取代的硝基苯甲化合物有利的电化学吸附在阴极表面的活性位置上,当阴极电势升高或槽电压较低时,烷基取代的硝基苯甲化合物脱附进入到电解液中。这样,化合物“电化学性可逆”,从而可以提供改进的氢气发生抑制。
通常,为本领域所熟知的,电容的阳极、阴极和工作电解液的物理设置可以变化。如图1所示,湿化电解电容40包括工作电解液44,位于阳极20和阴极43之间。阳极20包括绝缘膜21,其中插入导线42(如钽导线)。阴极43由多孔阴极基底41和电化学活性材料49形成,如上所述。虽然未示出,可以在阴极43和阳极20之间设置分离器以防止阳极和阴极直接接触,同时又允许离子从工作电解液44流向电极。已知的电解型中采用的任何作为分离器的材料都可以用作本发明的分离器。例如纸、塑料纤维、玻璃纤维、由这些纤维制成的纸、多孔膜以及离子能渗透的材料(如NafionTM)。通常,阳极和阴极间隔约10-约1000微米。在这一实施例中,多孔阴极基底41是圆柱形“听状”,并附有盖子。可以采用封条23(如玻璃-金属)连接并密封阳极20至阴极43。虽然未示出,电容40还可以包括间隔装置(未示出)以保持阳极20稳定在阴极43中。间隔装置可以由塑料制成,可以是垫圈形状。
本发明的电解电容器可以具有不同的应用,包括而不限于医疗器械,如心内除颤器、起搏器、心律转变器、神经刺激器、给药装置等;汽车应用;军事应用,如RADAR系统;消费性电子设备,如收音机、电视;等等。例如在一个实施例中,可以在设置成为病人提供治疗性高电压(如在约500-约850V之间,或者优选的在约600-约800V之间)的心内除颤器中使用电容器。该设备可以包括密封且生物惰性的容器或罩。一个或多个导线在设备及病人心脏间通过静脉电气连接。心脏电极用以感受心脏活动和/或为心脏提供电压。可以使至少部分导线(如导线端部分)邻近或接触一个或多个心室以及心房。该设备还包括电容层,其通常包括两个或多个串联的电容,它们与电池连接,该电池在设备以内或以外,为电容层提供能量。由于高电导率,本发明的电容能够达到优良的电气性能从而适用于可植入的医疗器械的电容层。例如,1000Hz频率的2V偏压和1V信号下等效串联电阻(ESR)——在电路中充电和放电时电容相当于电阻——可以低于约1500毫欧,在一些实施例中为低于约1000毫欧,在一些实施例中为低于约500毫欧。
通过以下实施例能够更好的理解本发明。
实施例1
根据本发明形成阴极的方法。一开始,1级钛薄片(厚度120μm,Sigma-Aldrich)切成宽度为10.0毫米的两个方块作为金属基底。方块用220号砂纸打磨以除去表面可见的瑕疵和污点。此后,在方块的上边缘中心点焊接一条15mm长的钽导线以方便后续过程和电气化测试。这些样品之后在超声波的肥皂浴中去油60分钟,用去离子水清洗5遍,之后在50℃和-26”汞柱的真空下干燥超过2小时。
为了形成多孔表面,这两个样品浸渍于1.0M硫酸溶液中。使用如上所述钛样品作为阳极以及铂网作为阴极形成电化学槽。以0.05A/cm2的密度通直流电穿过电化学电池以使金属基底阳极氧化。10分钟后,分离样品,用去离子水清洗5遍,在室温下干燥1小时。阳极化中使用的电压曲线如图2所示。如图所示,电压曲线包括两个不同的区域——氧化物膜形成区域(低于60V)和氧化物膜分解区域(高于60V)其中一个得到的多孔基底的照片如图3所示。如图所示,在电化学处理后形成网状结构,具有的孔径为约100-约1000纳米(0.1-1μm)。
之后在基底上涂敷M单体和CB催化剂以形成改性的聚(3,4-乙撑二氧噻吩)。使用乙醇清洗,在可控的室温下干燥超过2小时。为了确定阴极电容,采用标准圆柱钽阳极,并压缩至直径6.5mm高20.0mm。阳极阳极化以在120Hz频率下显示本征电容为2.62mF。导电聚合物涂敷的钛基底用作阴极。电解液为5.0M硫酸。使用4021Agilent LCR测量仪,使用Cs-Rs模式,偏压为2.0V,频率120Hz,交流电峰压值1.0V。采用下式计算阴极电容:
采用上式计算,两个样品的阴极电容分别为37.52mF/cm2和31.79mF/cm2。稳定性测试中,其中一个样品在70℃浸渍于pH为6.25的水性溶液。90天后PEDT涂层和金属基底未分层,也未出现PEDT颗粒脱离。
实施例2
如例1制备两个钛样品,在应用PEDT涂层之前修饰网结构,该网结构在750℃下氩气中热处理30分钟。得到的结构如图4所示。表面保持高度多孔,在一些部分出现孔径大于1000纳米(1μm)。样品的阴极电容分别为16.44mF/cm2和33.50mF/cm2。
实施例3
如例1制备两个钛样品,在应用PEDT涂层之前修饰网结构,该网结构在750℃下氩气中热处理30分钟,同时网结构表面有1g镁屑(magnesiumturnings)。得到的结构如图5所示。表面颜色由灰色变位黑色,可能是由于形成钛-镁合金。然而,如图所示,表面保持高度多孔和有序。样品的阴极电容分别为24.80mF/cm2和21.05mF/cm2。
实施例4
如例1制备四个钛样品,在应用PEDT涂层之前修饰网结构,该网结构在600℃下氩气中在石墨薄片(Alfa Aesar,平均尺寸为7-10μm)存在下热处理30分钟。得到的结构如图6所示。表面保持高度多孔和有序。样品的阴极电容分别为30.79mF/cm2、26.61mF/cm2、30.79mF/cm2和27.88mF/cm2。
实施例5
根据本发明制备阴极的方法。一开始,将1级钛薄片(厚度120μm,Sigma-Aldrich)切成宽度为10.0毫米的两个方块以作为金属基底。用220号砂纸打磨去除表面可见的瑕疵和污点。之后,在方块的上边缘中心点焊接一条15mm的钽导线以支持其后的过程和电气测试。这些样品之后在超声的肥皂浴中去油60分钟,用去离子水清洗5遍,之后在50℃和-26”汞柱的真空下干燥超过2小时。
为了形成多孔表面,两个样品浸渍于100ml的烧杯中,烧杯中为混合了11.3g磷酸、0.625g氯化氢、45ml乙二醇以及45ml去离子水的溶液。如上所述制得的钛样品作为阳极,铂网作为阴极得到电化学槽。以0.02A/cm2的密度通直流电穿过电化学槽以使金属基底阳极氧化。电流穿过电化学槽使电压达到25V并保持25V10分钟。10分钟后,分离样品,用去离子水清洗5遍,在室温下干燥1小时。之后样品在450℃空气中热处理1小时以达到从锐钛矿到金红石的相变。其中一个得到的多孔基底的照片如图7所示。如图所示,在电化学处理后形成管状结构,具有的孔径为约50-约300纳米(0.05-0.3μm)。基于生成常数2.8nm/V,管的预测深度为约70纳米。
实施例6
如例1制备两个钛样品,在应用PEDT涂层之前修饰网结构,该网结构在600℃下氢气中热处理30分钟,之后在700℃下真空(10-5torr)热处理20分钟。得到的结构如图8所示。表面保持高度多孔和有序。样品的阴极电容分别为36.36mF/cm2和32.46mF/cm2。
实施例7
如例1制备两个钛样品,在应用PEDT涂层之前修饰网结构,该网结构在200毫托的真空室中喷金15秒。样品的阴极电容分别为29.27mF/cm2和38.66mF/cm2。
实施例8
根据本发明制备阴极的方法。一开始,将钽薄片(厚度250μm,H.C.Starck)切成宽度为10.0毫米的两个方块以作为金属基底。用220号砂纸打磨去除表面可见的瑕疵和污点。之后,在方块的上边缘中心点焊接一条15mm的钽导线以支持其后的过程和电气测试。这些样品之后在超声的肥皂浴中去油60分钟,用去离子水清洗5遍,之后在50℃和-26”汞柱的真空下干燥超过2小时。
为了形成多孔表面,两个样品浸渍于由1.0M硫酸和10vol.%HF以体积比9∶1混合的溶液中。如上所述制得的钽样品作为阳极,铂网作为阴极得到电化学槽。以0.05A/cm2的密度通直流电穿过电化学槽以使金属基底阳极氧化。5分钟后,分离样品,用去离子水清洗5遍,在室温下干燥1小时。阳极化过程使用的电压曲线如图9所示。如图所示,压力曲线包括两个不同的区域——氧化物膜形成区域(低于100V)和氧化物膜分解区域(高于100V,110-140V)之后在基底上涂敷M单体和CB催化剂以形成改性的聚(3,4-乙撑二氧噻吩)。使用乙醇清洗,在室温下控制干燥过程超过2小时。得到的样品阴极电容为15.83mF/cm2和12.62mF/cm2。
实施例9
如例1制备一个钛样品,电化学活性材料不是PEDT而是电沉积的钯。在8.0g/L的PdCl2和1mol/L的HCl的混和液中进行浴处理。以铂网为阳极控制阴极电流强度为0.02A/cm2保持约40分钟。均匀的钯黑沉积在改性的钛表面。样品的阴极电容为5.46mF/cm2。
实施例10
如例1制备两个钛样品并面对面形成对称电容,其间以Celgard 3051聚丙烯隔离物分离。使用热收缩膜拉紧整个器件,并真空浸渍5.0M硫酸。电测试中,控制偏压0.6V,频率120Hz,交流电压峰压值10mV。电槽显现的电容值为12.0mF。
在不偏离本发明精神和范围的前提下,本领域的技术人员可以实行各种修饰或变形。此外,应力接到不同的实施方式间可以部分或全部代替互换。另外,本领域的技术人员应理解,上述实施方式只是示例性质,而不应限制本发明及权利要求书。
Claims (33)
1、一种湿化电容,包括:
阳极;
包括涂敷了电化学活性材料的阳极化金属基底的阴极,其中,基底包括在其表面形成的多个孔,所述孔的平均尺寸为约10-约1500纳米;以及位于阴极和阳极之间的工作电解液。
2、如权利要求1所述的湿化电容,其中,所述金属基底包括钛或钛合金。
3、如权利要求1所述的湿化电容,其中,所述孔的平均尺寸为约20-约1000纳米。
4、如权利要求1所述的湿化电容,其中,所述阳极化的基底在约20℃下具有约1×10-4ohm-cm或更小的电阻率。
5、如权利要求1所述的湿化电容,其中,所述孔的形状通常为管状。
6、如权利要求1所述的湿化电容,其中,所述孔占所述基底表面的约30%-约70%。
7、如权利要求1所述的湿化电容,其中,所述电化学活性材料包括导电聚合物。
8、如权利要求7所述的湿化电容,其中,所述导电聚合物包括聚(3,4-乙撑二氧噻吩)(poly(3,4-ethylenedioxythiophene))或其衍生物。
9、如权利要求1所述的湿化电容,其中,所述电化学活性材料包括金属颗粒、金属氧化物颗粒或它们的混合物。
10、如权利要求1所述的湿化电容,其中,所述工作电解液包括水性溶剂。
11、如权利要求1所述的湿化电容,其中,所述阳极包括钽、铌或它们的导电氧化物。
12、如权利要求1所述的湿化电容,其中,所述阳极为阳极化的,并包括绝缘膜。
13、如权利要求1所述的湿化电容,其中,所述阴极的比电容为约10mF/cm2或更高。
14、如权利要求1所述的湿化电容,其中,所述阴极的比电容为约25-约100mF/cm2。
15、如权利要求1所述的湿化电容,其中,所述阴极的厚度为约100微米或更低。
16、如权利要求1所述的湿化电容,其中,所述阴极的厚度为约10-约50微米。
17、如权利要求1所述的湿化电容,其中,所述基底进一步包括金属层。
18、一种导电阴极,包括涂敷了导电聚合物的阳极化金属基底,其中,所述基底包括在其表面形成的多个孔,所述孔的平均尺寸为约20-约1000纳米。
19、如权利要求18所述的阴极,其中,所述金属基底包括钛或其合金。
20、如权利要求18所述的阴极,其中,所述孔的平均尺寸为约50-约500纳米。
21、如权利要求18所述的阴极,其中,所述孔占所述基底表面的约30%-约70%。
22、如权利要求18所述的阴极,其中,所述导电聚合物包括聚(3,4-乙撑二氧噻吩)(poly(3,4-ethylenedioxythiophene))或其衍生物。
23、一种用于湿化电容的阴极的形成方法,包括:
将金属基底浸渍于阳极化溶液中;
在金属基底上应用第一电压下的电流以影响阳极氧化,并形成含有氧化物膜的阳极化基底;以及
使氧化物膜分解以在阳极化基底表面形成多个孔,所述孔的平均尺寸为约10-约1500纳米。
24、如权利要求23所述的方法,进一步包括将第一电压提高至第二电压,其中,第二电压大于第一电压,且为氧化物膜分解电压或更高。
25、如权利要求23所述的方法,进一步包括改变第一电压为第二电压,其中第二电压的极性与第一电压的极性相反。
26、如权利要求23所述的方法,其中,所述阳极化溶液包括离子化合物和腐蚀性化合物。
27、如权利要求23所述的方法,其中,所述金属基底包括钛或其合金。
28、如权利要求23所述的方法,其中,所述孔的平均尺寸为约20-约1000纳米。
29、如权利要求23所述的方法,进一步包括在阳极化基底上涂敷电化学活性材料。
30、如权利要求29所述的方法,其中,所述电化学活性材料包括导电聚合物。
31、如权利要求29所述的方法,其中,所述电化学活性材料包括金属颗粒、金属氧化物颗粒、或它们的组合。
32、如权利要求23所述的方法,其中,所述阳极化溶液的温度为约10℃-约50℃。
33、如权利要求23所述的方法,进一步包括以约200℃-约1400℃的温度在还原气氛下(reducing atmosphere)加热阳极化的基底。
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2009
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- 2009-06-24 DE DE102009027174A patent/DE102009027174A1/de not_active Withdrawn
- 2009-08-07 CN CN200910164879.2A patent/CN101673620B/zh not_active Expired - Fee Related
- 2009-09-02 JP JP2009202303A patent/JP2010067966A/ja not_active Ceased
- 2009-09-11 KR KR1020090086025A patent/KR20100031488A/ko not_active Application Discontinuation
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Also Published As
Publication number | Publication date |
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GB0909930D0 (en) | 2009-07-22 |
GB2464575A (en) | 2010-04-28 |
DE102009027174A1 (de) | 2010-04-15 |
KR20100031488A (ko) | 2010-03-22 |
US20100067174A1 (en) | 2010-03-18 |
US8023250B2 (en) | 2011-09-20 |
CN101673620B (zh) | 2014-03-19 |
JP2010067966A (ja) | 2010-03-25 |
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