CN101419866A - 用于形成电容器阳极的掺杂陶瓷粉末 - Google Patents
用于形成电容器阳极的掺杂陶瓷粉末 Download PDFInfo
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- CN101419866A CN101419866A CNA200810170997XA CN200810170997A CN101419866A CN 101419866 A CN101419866 A CN 101419866A CN A200810170997X A CNA200810170997X A CN A200810170997XA CN 200810170997 A CN200810170997 A CN 200810170997A CN 101419866 A CN101419866 A CN 101419866A
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- powder
- electrolytic capacitor
- capacitor
- anode
- niobium
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Abstract
本发明涉及用于形成电容器阳极的掺杂陶瓷粉末。在本发明的一种实施方案中提供了电解电容器,其包括由包含导电性陶瓷颗粒和含量为约百万分之100份或更多的非金属元素的粉末制成的阳极体。该非金属元素具有在三或更高的能级上包括五个价电子的基态电子构型。这种元素的实例包括例如磷、砷、锑等。该电容器还包括位于该阳极体之上的介电层和位于该介电层之上的电解质层。
Description
技术领域
本发明涉及用于形成电容器阳极的掺杂陶瓷粉末。
背景技术
电解电容器通常是由能够经氧化以形成介电层的阀作用材料制成。典型的阀作用金属是铌和钽。最近以来,已经开发了使用由导电性氧化铌(oxide niobium)和五氧化二铌(niobium pentoxide)介电体制备的阳极的电容器。基于氧化铌的电容器与钽电容器相比,具有显著的优点。例如,氧化铌比钽可更广泛地获得,而且可能处理成本更低。氧化铌电容器比钽和铌对进一步的氧化更稳定,因此在过压(或以其它方式过载)时较不容易热失控。此外,氧化铌具有比铌和钽高几个数量级的最小点火能量。氧化铌电容器也可能具有独特的高阻失效机理,这样会将泄漏电流限制到低于该电容器的热失控点之下的水平。
尽管这种陶瓷基(例如氧化铌)电容器提供了很多优点,但由于该介电体的较低击穿强度,使得其在高压应用(例如16、20或35伏特的额定电压)中的应用通常已经受到限制。一般而言,随着电容器上的电荷和电压的增加,自由电子最终将会在所谓雪崩击穿的过程中加速到能够在与中性原子或分子碰撞过程中释放其它电子的速度。击穿是非常突然发生的(通常在纳秒内),导致形成通过该材料的导电路径和击穿放电。在这种情况下可能发生电容器损坏或破坏。在氧化铌电容器中,我们相信Nb2O5-x的氧空位用作使阳极氧化物作为n型半导体的电子供体。不幸的是,我们相信Schottky型点缺陷在n型半导体中是占主导的,在n型半导体中氧原子离开其在晶格结构中的位置(由此产生氧空位),并移动到具有较低浓度的区域。在氧化铌电容器的情况下,我们相信在一氧化铌阳极和五氧化二铌介电体之间界面处的氧梯度驱动氧原子扩散到一氧化铌具有较低浓度的区域中,由此在介电体中产生氧空位。这些缺陷可能在介电体中形成深阱,其会将该电荷存储,并用作在DC电压作用下由Poole-Frenkel和隧道效应机理传递的电荷载体的来源。高电压和温度的作用进一步加速了氧的扩散,并增大了介电体中的缺陷数。这样导致在加速的温度和电压载荷下泄漏电流的不稳定性,其可能限制这种电容器在较高施加电压下的应用。
因此,目前存在对能够在较高电压下操作的由陶瓷基阳极(ceramic-based anode)形成的电解电容器的需求。
发明内容
依照本发明的一种实施方案,公开了电解电容器,其包括由包含导电性陶瓷颗粒和含量为约百万分之100份或更多的非金属元素的粉末制成的阳极体。该非金属元素具有在三或更高的能级包括五个价电子的基态电子构型。这种元素的实例包括例如磷、砷、锑等。该电容器还包括位于该阳极体之上的介电层和位于该介电层之上的电解质层。
依照本发明的另一实施方案,公开了用于形成电容器阳极的陶瓷粉末。该陶瓷粉末包含导电陶瓷颗粒,且具有约百万分之200份或更高的磷含量。在另一实施方案中,公开了电容器阳极的形成方法,其包括用磷掺杂剂掺杂导电陶瓷颗粒,以形成具有约百万分之200份或更高的磷含量的粉末。压制该粉末以形成压丸并烧结。
下面更详细地提出本发明的其它特征和方面。
附图说明
在参考附图的说明书的其余部分中,更特别地提出了对于本领域技术人员对本发明的完整和允许的公开,包括其最佳实施方案,其中:
图1是本发明的电解电容器的一种实施方案的透视图;
图2是图1的电容器沿2-2线的横截面视图;
图3是将电容器激光焊接到阳极端接的本发明的一种实施方案的示意图;和
图4是依照本发明的一种实施方案形成的激光焊接的电容器的横截面视图。
在本说明书和附图中附图标记的重复使用用于表示本发明的相同或类似的特征或要素。
具体实施方式
本领域的普通技术人员理解本讨论仅是示例性的实施方案的描述,并不意于限制本发明的更宽范围,该更宽范围体现在该示例性的结构中。
一般而言,本发明涉及用于形成电容器阳极的导电陶瓷粉末。该粉末通常具有高的荷质比,例如约25000微法拉*伏特/克(μF*V/g)或更高,在一些实施方案中为约40000μF*V/g或更高,在一些实施方案中为约60000μF*V/g或更高,在一些实施方案中为约70000μF*V/g或更高,在一些实施方案中为约80000~约200000μF*V/g或更高。用于形成这种粉末的陶瓷颗粒的实例包括阀金属(例如钽、铌等)的氧化物。一种特别有效类型的适用于本发明的陶瓷颗粒是导电性的铌氧化物,例如具有1:小于2.5,在一些实施方案中为1:小于1.5,在一些实施方案中为1:1.0±0.1,在一些实施方案中为1:1.0±0.05的铌/氧原子比的铌氧化物。例如该铌氧化物可以是NbO0.7、NbO1.0、NbO1.1和NbO2。在优选实施方案中,该陶瓷颗粒包含为导电铌氧化物的NbO1.0,其甚至可以在高温烧结之后仍保持化学稳定。在Fife的美国专利号6322912、Fife等的6391275、Fife等的6416730、Fife的6527937、Kimmel等的6576099、Fife等的6592740、和Kimmel等的6639787、和Kimmel等的7220397、以及Schnitter的美国专利申请公开号2005/0019581、Schnitter等的2005/0103638、Thomas等的2005/0013765中都描述了这种阀金属氧化物的实例,此处为了所有目的将所有这些都通过参考整体引入此文。
陶瓷颗粒可以具有任意所需的形状或尺寸。例如,该颗粒可以是薄片状、棱角状、结节状及其混合或变体形状。颗粒通常也具有至少约60目的筛分粒度分布,在一些实施方案中为约60~约325目,在一些实施方案中为约100~约200目。此外,比表面积为约0.1~约10.0m2/g,在一些实施方案中为约0.5~约5.0m2/g,在一些实施方案中为约1.0~约2.0m2/g。术语“比表面积”是指由Bruanauer,Emmet和Teller,Journal ofAmerican Chemical Society,Vol.60,1938,p.309的物理气体吸附(B.E.T.)方法测定的表面积,使用氮气作为吸附气体。同样地,堆积(或Scott)密度通常为约0.1~约5.0克/立方厘米(g/cm3),在一些实施方案中为约0.2~约2.5g/cm3,在一些实施方案中为约0.5~约1.5g/cm3。
依照本发明,陶瓷粉末也包含“非金属元素”,其包括真正的非金属(例如磷)以及准金属,例如可以形成两性氧化物和/或表现为半金属的元素(例如锑)。非金属元素具有在三(3)或更高的能级包括五(5)个价电子的基态电子构型。不希望被理论限制,我们相信这种电子构型可以为该元素提供与自由氧电子键合并由此阻止它们从介电体到陶瓷阳极的运动的能力。这种电子构型也被认为使该元素容易溶解在具有五(5)个价电子的介电基质(例如Nb2O5或Ta2O5)中。
用于本发明的阳极的合适非金属元素可以包括例如磷、锑、砷等。例如,磷具有1s22s22p63s23px 13py 13pz 1的基态电子构型。为了形成五(5)个共价键,可以将3s轨道的一个电子激发成3d轨道的一个电子。3能级电子自身杂化得到5个杂化轨道,所有的具有等能量(即dsp3杂化轨道),其可以与来自五(5)个氧原子的电子共享空间,以形成五(5)个新分子轨道,由此形成五(5)个共价键。与磷类似,锑和砷都具有在“s”轨道中包含可以激发到更高能态的电子的电子构型。例如,砷在4s轨道包含可以激发到4d轨道的电子,然后其杂化成五(5)个dsp3杂化轨道。类似地,锑在5s轨道包含可以激发到5d轨道的电子,然后其杂化成五(5)个dsp3杂化轨道。另一方面,氮具有1s22s22px 12py 12pz 1的电子构型。因为从2s能级到3s能级的能量差距通常大,因此通常不会发生2s电子的激发,这意味着氮通常不会形成五(5)个共价键。
该非金属元素通常通过掺杂剂引入该陶瓷粉末中。任何能够释放所需浓度的该非金属元素且对该粉末的电性质没有显著不利影响的掺杂剂都可以适用于本发明。在一种实施方案中,例如,该掺杂剂可以是包含至少一种金属(例如钽、铌、铝、镓、铟、铊(thalium)等)和至少一种非金属元素(例如磷、砷和锑)的化合物。一类适用于本发明的掺杂剂是金属磷化物,其可以以粉末形式提供,并因此容易与陶瓷颗粒混合。示例性的金属磷化物包括例如磷化铁、磷化锌、磷化钛、磷化锰、磷化锡、磷化铜、磷化镍、磷化钽、磷化铬、磷化铌、磷化锂、磷化钠、磷化镁、磷化镉、磷化钼、磷化钨、磷化钒、磷化锆、磷化钴、磷化铪、磷化钡、磷化硼、磷化铝、磷化镓、磷化铟、磷化铱、磷化钪、磷化钇、磷化镧、磷化铈、磷化镨、磷化铽、磷化铒、磷化镝、磷化钬、磷化钕、磷化钐、磷化锗、磷化钙、磷化银、磷化铂、磷化钆、磷化铝镓、磷化镓铟、磷化铝镓铟、磷化镓铟砷等。当由铌氧化物形成陶瓷颗粒时,可能特别希望使用磷化铌作为掺杂剂以提高该掺杂剂和陶瓷颗粒的相容性。
当然,在本发明中也可以使用其它掺杂剂。在某些实施方案中,例如,该掺杂剂可以是磷酸,及其盐或酯比如磷酸铵、磷酸镓、烷基磷酸酯等。磷也可以以磷酸和其它化合物(例如包含氮的碱性有机化合物,例如氨、伯和仲胺、环胺、吡啶族化合物和喹啉类和吡咯族化合物)的混合物的形式引入。
可以使用多种技术将掺杂剂引入该粉末中。例如,在一种实施方案中,将掺杂剂和该导电陶瓷颗粒简单混合。可替代地,可以将掺杂剂施加到起始材料(例如Nb2O5)上,然后在吸气材料(例如钽或铌)的存在下对其进行热处理以形成氧还原的和导电性的陶瓷(NbO)。热处理通常发生在便于氧原子从起始氧化物传递到该吸气材料的气氛中。例如,该热处理可以发生在还原气氛中,例如在真空、惰性气体、氢气等中。该还原气氛的压力可以为约10托~约2000托,在一些实施方案中为约100托~约1000托,在一些实施方案中为约100托~约930托。通常,热处理的发生温度为约800℃~约1900℃,在一些实施方案中为约1000℃~约1500℃,在一些实施方案中为约1100℃~约1400℃,热处理时间为约5分钟~约100分钟,在一些实施方案中为约30分钟~约60分钟。
为了达到介电性质的所需改进,该非金属元素的含量为约百万分之(“ppm”)100份或更高,在一些实施方案中为约200ppm或更高,在一些实施方案中为约400ppm或更高,在一些实施方案中为约500ppm或更高,在一些实施方案中为约800ppm或更高,在一些实施方案中为1000ppm或更高,在一些实施方案中为约1500ppm到约10000ppm,在一些实施方案中为约3000ppm~约5000ppm。已经发现甚至在这么高的水平下,所述非金属元素仍不会显著阻碍该陶瓷颗粒的烧结活性。
为了便于形成阳极,在将陶瓷颗粒和掺杂剂混合在一起之前或之后,也可以在陶瓷颗粒或掺杂剂中添加其它组分。例如,将陶瓷颗粒和掺杂剂可以非必要地与粘结剂和/或润滑剂相混合以确保颗粒在压紧以形成阳极体时充分彼此粘合。适合的粘结剂可以包括樟脑、硬脂酸和其它肥皂质脂肪酸、Carbowax(Union Carbide)、Glyptal(General Electric)、聚乙烯醇、萘(napthaline)、植物蜡和微晶蜡(精制石蜡)。该粘结剂可以溶解和分散在溶剂中。示例性的溶剂可以包括水、醇等。在使用时,粘结剂和/或润滑剂的百分比可以在总物质重量的约0.1wt%~约8wt%之间变化。然而,应当理解粘结剂和润滑剂在本发明中并不是必需的。
一旦形成,可以使用任何常用的粉末压模将粉末压实。例如,该压模可以是使用模具和一个或多个冲杆的单站压模(single stationcompaction press mold)。可替代地,可以使用仅使用模具和单下冲杆的铁砧型压模。单站压模可以几种基本形式获得,例如具有不同性能的凸轮(cam)、肘节/肘杆(toggle/knuckle)和偏心/曲柄压机(eccentric/crankpress),例如单动、双动、浮沉模(floating die)、动压板(movable platen)、对置柱塞(opposed ram)、螺杆(screw)、冲击、热压、压印(coining)或上胶(sizing)。该粉末可以压实在阳极线(例如钽线)周围。应当进一步认识到该阳极线可以替代地连接(例如焊接)到阳极体上,这在压制和/或烧结该阳极体之后进行。在压实之后,可以通过在真空下在特定温度下(例如约150℃~约500℃)将丸粒加热数分钟来去除任何粘结剂/润滑剂。可替代地,也可以通过使该丸粒与含水溶液接触来去除该粘结剂/润滑剂,例如Bishop等的美国专利号6197252中所述,为了所有目的将其通过参考整体引入此文。然后,将该丸粒烧结以形成多孔的完整块。例如,在一种实施方案中,可以在约1200℃~约2000℃,在一些实施方案中约1500℃~约1800℃的温度下在真空下烧结该丸粒。烧结时,由于颗粒之间键的生长,该丸粒收缩。除上述技术之外,依照本发明也可以使用任何其它用于形成阳极体的技术,例如Galvagni的美国专利号4085435、Sturmer等的4945452、Galvagni的5198968、Salisbury的5357399、Galvagni等的5394295、Kulkarni的5495386和Fife的6322912中所述,为了所有目的将其通过参考整体引入此文。
尽管不要求,但可以选择阳极体的厚度以改进该电容器的电性能。例如,该阳极体的厚度可以为约4毫米或更小,在一些实施方案中为约0.2~约3毫米,在一些实施方案中为约0.4~约1毫米。这种相对较小的阳极厚度(即“低外形”)有助于消散高荷质比粉末产生的热量,还为使ESR和电感的最小化提供了更短的传输路径。也可以选择阳极体的形状以改进所得到的电容器的电性质。例如,该阳极体可以具有弯曲、正弦曲线、矩形、U形、V形等的形状。该阳极体也可以具有“槽形”形状,其中其包含一个或多个沟槽、凹槽、凹陷或压痕,以提高表面和容积之比,以使ESR最小化并延长电容器的频率响应。在例如Webber等的美国专利号6191936、Maeda等的5949639和Bourgault等的3345545以及Hahn等的美国专利申请公开号2005/0270725中描述了这种“槽形”阳极,为了所有目的将其所有都通过参考整体引入此处。
一旦形成,可以对该阳极进行阳极化,以在该阳极上和内部形成介电层。阳极化是电化学工艺,通过其将该阳极氧化以形成具有较高介电常数的材料。例如,可以对氧化铌(NbO)阳极进行阳极化以形成五氧化二铌(Nb2O5)。特别地,在一种实施方案中,在用受控电压和电流提供的升高温度下(例如约85℃),将该氧化铌阳极浸入弱酸溶液(例如磷酸、多磷酸、其混合物等)中形成具有一定厚度的五氧化二铌涂层。粉末供给最初保持在恒定的电流,直到达到所需的形成电压。然后,将粉末供给保持在恒定的电压下,以确保在阳极表面上形成所需的介电层厚度。该阳极化电压通常在约10~约200伏特,在一些实施方案中在约20~约100伏特的范围内。除了在阳极表面上形成之外,通常在该材料的孔表面上也形成一部分介电氧化物膜。应当理解该介电层可以由其它类型的材料和使用不同的技术形成。
一旦形成介电层,可以非必要地施加保护涂层,例如由相对绝缘的树脂类材料(天然或合成)形成的。这种材料可以具有大于约0.05欧姆-cm,在一些实施方案中大于约5,在一些实施方案中大于约1000欧姆-cm,在一些实施方案中大于约1×105欧姆-cm,在一些实施方案中大于约1×1010欧姆-cm的电阻系数。可以用于本发明的一些树脂类材料包括但不局限于聚氨酯、聚苯乙烯、不饱和或饱和脂肪酸的酯(例如甘油酯)等。例如,适合的脂肪酸酯包括但不局限于月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、桐酸、油酸、亚油酸、亚麻酸、紫胶桐酸、紫胶酸等的酯。发现这些脂肪酸酯在以相对复杂的组合使用以形成“干性油”的时候是特别适用的,其使所得到的膜快速聚合成稳定层。这种干性油可以包括单、二和/或三甘油酯,其具有甘油主链,该甘油主链分别具有一个、两个和三个酯化的脂肪酰基残基。例如,可以使用的一些适合的干性油包括但不局限有橄榄油、亚麻子油、蓖麻油、桐油、大豆油和虫胶。在Fife等的美国专利号6674635中对这些和其它保护性涂层材料做了更详细的描述,为了所有目的将其通过参考整体引入此处。
然后将该阳极化部分经历依照常规技术形成阴极的步骤。在一些实施方案中,例如,通过将硝酸锰(Mn(NO3)2)热解以形成二氧化锰(MnO2)阴极来形成阴极。在例如Sturmer等的美国专利号4945452中描述了这种技术。为了所有目的将其通过参考整体引入此处。可替代地,可以使用导电聚合物涂层来形成该电容器的阴极。导电聚合物涂层可以包括一种或多种导电聚合物,例如聚吡咯、聚噻吩(例如聚(3,4-亚乙二氧基噻吩)(PEDT))、聚苯胺、聚乙炔、聚-对-亚苯基及其衍生物。而且,如果需要,也可以由多种导电聚合物层形成该导电聚合物涂层。例如,在一种实施方案中,该导电聚合物涂层可以包含由PEDT形成的一层和由聚吡咯形成的另一层。可以使用各种方法在该阳极部分上涂覆导电聚合物涂层。例如,可以使用常规技术,例如电聚合、丝网印刷、浸渍、电泳涂覆和喷涂,形成导电聚合物涂层。在一种实施方案中,例如,可以首先将用于形成该导电聚合物的单体(例如3,4-亚乙二氧基噻吩)与聚合催化剂混合形成溶液。例如,一种适合的聚合催化剂是BAYTRONC,其是甲苯-磺酸铁III,由H.C.Starck销售。BAYTRON C是用于BAYTRON M的市场上可得到的催化剂,BAYTRON M是3,4-亚乙二氧基噻吩,也由H.C.Starck销售的PEDT单体。一旦形成催化剂分散体,然后可以将该阳极部分浸入该分散体中以在该阳极部分的表面上形成聚合物。可替代地,也可以将该催化剂和单体分别施加到该阳极部分上。在一种实施方案中,例如,可以将该催化剂溶解在溶剂(例如丁醇)中,然后作为浸渍溶液施加到该阳极部分上。然后可以干燥该阳极部分以从其上去除溶剂。然后,该阳极部分可以浸渍到包含适合单体的溶液中。一旦该单体接触包含催化剂的阳极部分的表面,就在其上进行化学聚合。除此之外,可以将该催化剂(例如BAYTRON C)与用于形成非必要的保护性涂层的材料(例如树脂类材料)混合。在这种情况下,然后可以将该阳极部分浸渍到包含该导电单体(BAYTRON M)的溶液中。因此,该导电单体可以接触在该保护性涂层的表面内部和/或之上的催化剂,并与其反应以形成导体聚合物涂层。尽管上面描述了多种方法,但应当理解在本发明中也可以使用任何其它用于在阳极部分上施加导电涂层的方法。例如,在Sakata等的美国专利号5457862、Sakata等的5473503、Sakata等的5729428和Kudoh等的5812367中可以描述了其它用于施加这种导电聚合物涂层的方法,为了所有目的将其通过参考整体引入此处。
在大多数实施方案中,一旦经过施加,该导体聚合物就恢复(heal)。恢复可以发生在导电聚合物层的每次施加之后或者可以发生在整个导电聚合物涂层的施加之后。在一些实施方案中,例如,可以通过将该丸粒浸渍到电解质溶液(例如磷酸和/或硫酸溶液)中,然后对该溶液施加恒定电压直至该电流降低到预设水平来恢复该导体聚合物。如果需要,这种恢复可以以多步完成。例如,在一种实施方案中,首先将具有导电聚合物涂层的丸粒浸渍到磷酸中并施加约20伏特,然后浸渍到硫酸中并施加约2伏特。在此实施方案中,第二低压硫酸溶液或甲苯磺酸的应用可以有助于提高电容并降低所得到的电容器的耗散因子(DF)。在施加上述一些或所有层后,如果需要,然后可以洗涤该丸粒,以去除各种副产物、过量的催化剂等。此外,在一些情况中,在上述一些或所有浸渍操作之后可以采用干燥。例如,在施加催化剂之后和/或在洗涤丸粒之后可能需要干燥,以打开该丸粒的孔以使其在随后的浸渍步骤过程中能够接受液体。
一旦阴极形成,该部分可以非必要地施加有碳层(例如石墨)和银层。例如,银涂层可以充当用于该电容器元件的可钎焊的导体、接触层和/或电荷收集器,碳涂层可以限制银涂层和电解质的接触。这种涂层可以覆盖电解质的一些或所有。
然后可以使用本领域的已知技术对所得到的电容器元件进行端接(terminate)。参照图1-2,例如,示出了电容器元件30的一种实施方案,其具有通常为矩形的形状,且分别包含前表面36、后表面38、顶表面和底表面37和39、和侧表面32(仅示出其中之一)。阳极线34从该电容器元件30的前表面36纵向(“y”方向)延伸。如图2中进一步所示,该电容器元件30包含阳极体50、位于该阳极体50之上的介电层52、位于该介电层52之上的固体电解质层54、位于该有机固体电解质层54之上的石墨层56、和位于该石墨层56之上的银层58。当然,应当理解这些层可以施加到该电容器的任意表面,并且不必需以所示方式施加。
一旦形成该电容器元件30,可以将阳极和阴极终端分别电连接到该阳极线34和固体电解质层54(经过石墨和银层)。该终端的特定构造可以如本领域中公知的那样变化。参照图3,例如,示出了一种实施方案,其包括阳极终端70和阴极终端80。在该特定的实施方案中,该阴极终端包含基本和第二部分84垂直的第一部分82。该第一部分82与电容器元件30的下表面39电接触,第二部分84与该电容器元件30的后表面38电接触。为了将该电容器元件30与该阴极终端80相连接,可以如本领域中已知的那样使用导电性粘结剂。例如,该导电性粘结剂可以包括用树脂组合物包含的导电性金属颗粒。该金属颗粒可以是银、铜、金、铂、镍、锌、铋等。该树脂组合物可以包含热固性树脂(例如环氧树脂)、固化剂(例如酸酐)和偶合剂(例如硅烷偶合剂)。Osako等的美国专利申请公开号2006/0038304中描述了适合的导电性粘结剂,为了所有目的将其通过参考整体引入此处。
阳极终端70包含几乎与第二部分74垂直的第一部分76。该第二部分74包含支撑阳极线34的区域。在所示的实施方案中,该区域51具有“U形形状”,用于进一步提高该线34的表面接触和机械稳定性。然后用激光90将该阳极线34焊接到区域51上。一旦该电容器元件与该终端相连接,将其封闭在树脂外壳内,然后可以用二氧化硅或其它任何已知的封装材料对其填充。该外壳的宽度和长度可以根据预期的应用而变化。然而,该外壳的总厚度通常小,以使所得到的组件可以容易地结合到低外形产品(例如“IC卡”)中。例如,该外壳的厚度可以在约4.0毫米或更小,在一些实施方案中为约0.1~约2.5毫米,在一些实施方案中在约0.15~约2.0毫米的范围内。适合的外壳可以包括例如“A”、“B”、“H”或“T”外壳(AVX Corporation)。参照图4,例如,示出了用于电容器组件100的这种封装外壳的一种特定的实施方案,示为元件88。该封装外壳88为该电容器组件100提供了另外的结构和热保护。在封装之后,可以将各阳极和阴极终端的暴露部分进行老化、遮蔽和修整。如果需要,该暴露部分可以非必要的沿该外壳88的外面弯曲两次(例如以约90°角)。
作为本发明的结果,可以形成具有优秀电性质的电容器。例如,本发明的电容器通常具有小于约1000毫欧姆(mohm),在一些实施方案中小于约500mohm,在一些实施方案中小于约100mohm的ESR。电容器的等效串联电阻通常是指在电路中充放电时该电容器充当电阻器的程度,通常表示为与该电容器串连的电阻。另外,通常表示从一个导体通过绝缘体流向相邻导体的电流的合成泄漏电流可以保持在较低的水平。例如,本发明的电容器的标称泄漏电流的数值在一些实施方案中小于约0.1μA/μF*V,在一些实施方案中小于约0.01μA/μF*V,在一些实施方案中小于约0.001μA/μF*V,其中μA是微安培,μF*V是电容和额定电压的乘积。同样地,本发明的电容器的击穿电压可以为至少约10伏特,在一些实施方案中至少约15伏特,在一些实施方案中至少约20伏特,在一些实施方案中为约20伏特~约100伏特。可以通过在恒定电流下以0.5伏特的增量提高施加电压来测定电容器的击穿电压。电容器损坏的电压为击穿电压。
参照以下实施例,本发明可以得到更好的理解。
测试程序
等效串连电阻(ESR)、电容和耗散因子:
使用具有0伏特偏差和1伏特信号的Kelvin Leads的Keithley 3330Precision LCZ仪器测定等效串连电阻和阻抗。操作频率为100kHz。使用具有2伏特偏差和1伏特信号的Kelvin Leads的Keithley 3330Precision LCZ仪器测定电容和耗散因子。操作频率为120Hz,温度为23℃±2℃。
泄漏电流:
使用由Mantracourt Electronics LTD,UK制造的MC 190 Leakage测试装置测定泄漏电流(“DCL”)。MC 190测试在25℃的温度和在10秒后的特定额定电压下测定泄漏电流。
寿命测试:
对于电容器的寿命测试,将其钎焊在测试板上,并放入处于Vc(0.66×Vr=0.66×16V=10.6V)和温度(125℃)的炉子中。测定测试前后的泄漏电流。如果该值高于特定的预设限(例如1μA),那么将该样品标为“不合格”-“rej.”。如果该值高于短路限(例如179μA),那么将该样品标为“SC”。
实施例1
将NbO粉末(HC Starck,80000μF*V/g)与磷化铌(325目,Alfa Aesar)手动混合获得100、200、500、1000ppm的最终磷浓度。将所得到的掺杂粉末在粉末混合机中均化。在该干粉末中添加含水溶液,该含水溶液包含聚乙基噁唑啉(“PX”)粘结剂(基于掺杂NbO粉末干重为2wt%的PX)。手动将该粘结剂溶液和掺杂粉末混合在一起。然后,将该粉末在85℃干燥4小时以使水分蒸发。然后钽引线和该粉末包埋,并在上/下压床上压实到3.4g/cm3的密度。然后通过将该丸粒放入400℃~500℃温度下的氮气气氛中,去除粘结剂。然后在氩气气氛中将该丸粒在1520℃的温度下烧结10分钟。
为使钽阳极阳极化,将其浸渍在具有8.6±0.3mS/cm的电导率和85±5℃的温度的弱磷酸/水溶液中,施加65V电压和高于100mA/g的电流,用去离子水清洗。然后如本领域中已知的那样对整个部件施加二氧化锰阴极层。然后,将该部件在室温下浸渍到石墨分散体中,在125℃恢复30分钟。然后将该部件在室温下浸渍到银分散体中,在125℃恢复30分钟。一旦该电容器元件形成,然后将其用激光焊接到具有0.10毫米厚度的引线框架(NILO作为原料)上。阳极线的直径为0.17毫米。使用银负载粘结剂ACE 10131(Protavic)连接阴极终端引线(引线框架的相对部分)。将该粘结剂在175℃固化1分钟。一旦该电容器元件连接到该引线框架上,然后将其封装以生成标准A外壳尺寸(AVX)电容器,并在170℃固化60秒。
一旦形成,测量各种电参数,使用25个电容器进行寿命测试。结果如下所示。
磷含量[ppm] | DCL[μA] | 寿命测试后DCL的不合格数 |
0 | 0.355 | 23rej |
100 | 0.394 | 25rej |
200 | 0.176 | 12rej |
500 | 0.229 | 9rej |
1000 | 0.173 | 2rej |
如上所示,较高的磷含量改进了电容器的泄漏电流稳定性。
实施例2
如实施例1所述相同方式形成电容器,只是原料NbO(N)粉末包含3000ppm的氮。一旦形成,测量各种电参数,使用25个电容器进行寿命测试。结果如下所示。
氮含量[ppm] | 磷含量[ppm] | DCL[μA] | 寿命测试后DCL的不合格数 |
3000 | 0 | 0.101 | 25rej |
3000 | 100 | 0.045 | 25rej |
3000 | 200 | 0.120 | 25rej |
3000 | 500 | 0.001 | 25rej |
3000 | 1000 | 0.053 | 25rej |
用磷掺杂的NbO粉末显示了比实施例1更低的DCL结果。预期更高的磷浓度液也会导致DCL稳定性的提高。
实施例3
如实施例1所述相同方式形成电容器,只是原料NbO粉末包含5000ppm的氮。一旦形成,测定各种电参数,使用25个电容器进行寿命测试。结果如下所示。
氮含量[ppm] | 磷含量[ppm] | DCL[μA] | 寿命测试后DCL的不合格数 |
5000 | 0 | 0.101 | 25rej |
5000 | 100 | 0.045 | 25rej |
5000 | 200 | 0.120 | 25rej |
5000 | 500 | 0.001 | 25rej |
5000 | 1000 | 0.053 | 25rej |
实施例4
如实施例1所述相同方式形成电容器,只是原料NbO粉末具有60000μF*V/g的荷质比。一旦形成,测定各种电参数,使用25个电容器进行寿命测试。结果如下所示。
磷含量[ppm] | DCL[μA] | 寿命测试后DCL的不合格数 |
0 | 0.297 | 23rej |
100 | 0.844 | 25SC |
200 | 0.756 | 25SC |
500 | 0.361 | 25SC |
1000 | 0.704 | 25rej |
本领域的普通技术人员在不脱离本发明的精神和范围的情况下可以实施本发明的这些和其它改变和变化。此外,应当理解各种实施方案的方面可以全部或部分互换。此外,本领域的普通技术人员将认识到前述描述仅是实施例的方式,并不意于限制本发明,在后附权利要求中将对其进行进一步的描述。
Claims (25)
1.电解电容器,包括:
由包含导电性陶瓷颗粒和含量为约百万分之100份或更多的非金属元素的粉末制成的阳极体,该非金属元素具有在三或更高的能级上包括五个或更多个价电子的基态电子构型;
位于该阳极体之上的介电层;和
位于该介电层之上的电解质层。
2.权利要求1的电解电容器,其中该陶瓷颗粒包含铌、钽、钒的氧化物或其组合。
3.权利要求1的电解电容器,其中该陶瓷颗粒包含具有约1:小于1.5的铌/氧原子比的铌氧化物。
4.权利要求1的电解电容器,其中该陶瓷颗粒包含具有1:1.0±0.1的铌/氧原子比的铌氧化物。
5.权利要求1的电解电容器,其中该粉末具有约80000μF*V/g或更高的荷质比。
6.权利要求1的电解电容器,其中该非金属元素包括磷、砷、锑或其组合。
7.权利要求6的电解电容器,其中该非金属元素包括磷。
8.权利要求6的电解电容器,其中该非金属元素在该粉末中的含量为约百万分之200份或更多。
9.权利要求6的电解电容器,其中该非金属元素在该粉末中的含量为约百万分之1000份~约百万分之5000份。
10.权利要求1的电解电容器,进一步包括至少一个位于电解质层之上的其它层,该其它层包括碳层、银层或其组合。
11.权利要求1的电解电容器,进一步包括从该阳极体伸出的阳极导线。
12.权利要求11的电解电容器,进一步包括:
与该电解质层电连接的阴极端接;
与该阳极体电连接的阳极端接;和
封装该电容器并保留至少一部分该阳极和阴极端接暴露的外壳。
13.权利要求1的电解电容器,其中该电解质层包含导电聚合物。
14.权利要求1的电解电容器,其中该电解质层包含二氧化锰。
15.权利要求1的电解电容器,其中该电容器的击穿电压至少为约16伏特。
16.用于形成电容器阳极的陶瓷粉末,该陶瓷粉末包含导电陶瓷颗粒,该粉末具有约百万分之200份或更高的磷含量。
17.权利要求16的粉末,其中该陶瓷颗粒包含具有1:1.0±0.1的铌/氧原子比的铌氧化物。
18.权利要求16的粉末,其中该粉末具有约25000μF*V/g或更高的荷质比。
19.权利要求16的粉末,其中该磷含量为约百万分之500份或更高。
20.权利要求16的粉末,其中该磷含量为约百万分之1000份~约百万分之5000份。
21.电容器阳极的形成方法,该方法包括:
用磷掺杂剂掺杂导电陶瓷颗粒,以形成具有约百万分之200份或更高的磷含量的粉末;
压实该粉末以形成压制的丸粒;和
烧结该压制的丸粒。
22.权利要求21的方法,进一步包括在压实之前将该粉末与粘结剂混合。
23.权利要求21的方法,其中该掺杂剂包括金属磷化物。
24.权利要求23的方法,其中该金属磷化物包括磷化铌。
25.权利要求24的方法,其中该陶瓷颗粒包含具有1:1.0±0.1的铌/氧原子比的铌氧化物。
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JP (1) | JP2009105406A (zh) |
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CN (1) | CN101419866B (zh) |
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CN115287737A (zh) * | 2022-08-03 | 2022-11-04 | 昆明理工大学 | 一种钛基梯度复合二氧化锰阳极板及其制备方法 |
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2008
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- 2008-08-12 DE DE102008041169A patent/DE102008041169A1/de not_active Withdrawn
- 2008-10-07 KR KR1020080098018A patent/KR20090040842A/ko not_active Application Discontinuation
- 2008-10-21 CN CN200810170997XA patent/CN101419866B/zh not_active Expired - Fee Related
- 2008-10-22 JP JP2008271725A patent/JP2009105406A/ja active Pending
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101814380A (zh) * | 2009-02-20 | 2010-08-25 | 阿维科斯公司 | 包含非金属表面处理的固体电解电容的阳极 |
CN101814380B (zh) * | 2009-02-20 | 2014-04-02 | Avx公司 | 包含非金属表面处理的固体电解电容的阳极 |
CN107077972A (zh) * | 2014-09-15 | 2017-08-18 | 凯米特电子公司 | 具有聚合物阴极的钽电容器 |
CN107077972B (zh) * | 2014-09-15 | 2019-06-28 | 凯米特电子公司 | 具有聚合物阴极的钽电容器 |
CN115287737A (zh) * | 2022-08-03 | 2022-11-04 | 昆明理工大学 | 一种钛基梯度复合二氧化锰阳极板及其制备方法 |
Also Published As
Publication number | Publication date |
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GB0814675D0 (en) | 2008-09-17 |
HK1128814A1 (en) | 2009-11-06 |
KR20090040842A (ko) | 2009-04-27 |
CN101419866B (zh) | 2012-02-22 |
US7760487B2 (en) | 2010-07-20 |
GB2454049B (en) | 2011-10-26 |
US20090103247A1 (en) | 2009-04-23 |
GB2454049A (en) | 2009-04-29 |
DE102008041169A1 (de) | 2009-04-30 |
JP2009105406A (ja) | 2009-05-14 |
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