CN100441515C - 铌低价氧化物粉末 - Google Patents

铌低价氧化物粉末 Download PDF

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CN100441515C
CN100441515C CNB2004100698999A CN200410069899A CN100441515C CN 100441515 C CN100441515 C CN 100441515C CN B2004100698999 A CNB2004100698999 A CN B2004100698999A CN 200410069899 A CN200410069899 A CN 200410069899A CN 100441515 C CN100441515 C CN 100441515C
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niobium
niobium suboxide
suboxide
powder
content
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O·托马斯
C·施尼特
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Tantalum Niobium Obisheng Innovative Materials Co Ltd
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HC Starck GmbH
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Abstract

含有100至600ppm镁及/或50至400ppm钼及/或钨的铌低价氧化物粉末，它适合于制造具有铌五氧化物绝缘材料层的电容器、由此铌低价氧化物粉末制得的电容器阳极以及相应的电容器。

Description

铌低价氧化物粉末
本发明涉及铌低价氧化物粉末，它适合于制造有铌五氧化物绝缘材料层的电容器，涉及由此铌低价氧化物粉末制造的电容器阳极，并涉及相应的电容器。
固体电解质电容器有效电容器表面积很大，因此总体结构小，适合于移动通讯所用的电子设备，是流行的电容器具有敷涂至相应导电衬底上之铌或钽五氧化物绝缘层，它利用了这些化合物(“阀门金属”)的稳定性、相对高的介电常数以及实际上该绝缘五氧化物层能通过电化学法以十分均匀的层厚度来加以制备的性质。所用衬底为该相应五氧化物的金属的或导电性的低价氧化物母体。此同时形成电容器电极(阳极)的衬底有高度多孔的海绵状结构，它通过烧结已呈海绵状的极细颗粒初级或次级构造而产生。此衬底构件表面被电解氧化(“形成”)以产生该五氧化物，该五氧化物层的厚度由电解氧化的最高电压(“形成电压”)确定。对电极是通过以热转换为二氧化锰的硝酸锰浸渍该海绵状构件而制得，或者以聚合物电解质液体产物母体浸渍接着进行聚合而制得。借助于衬底构件制造过程中烧结的钽或铌丝在一侧上形成至电极的电连接，而在另一侧上则形成金属电容器壳层，它对该丝绝缘。
电容器的电容C用下列公式来计算：
C＝(F·ε)/(d·VF)
式中F代表电容器的表面积，ε为介电常数，d为每伏形成电压的绝缘材料层的厚度，而VF为形成电压。由于对于钽五氧化物或铌五氧化物，介电常数ε分别为2 7.6或41，而且每伏形成电压的层厚度增长d为16.6或25
Figure C20041006989900031
所以两种五氧化物的上述系数ε/d分别等于1.64或1.69。基于两种五氧化物的电容器，由于阳极结构的几何形状相同，因此具有相同的电容。与比重有关之电容的细微具体差别由Nb、NbOx和Ta的不同密度所引起。阳极构件由Nb和NbOx制得，因此当使用时有节省重量的优点，例如在移动电话中，其中每节省一克重量都是优先考虑的事。关于成本方面，NbOx比Nb更为可取，因为阳极构件的某些体积由氧提供。
EP 1 388 870 A1已披露，一种通过烧结分子式NbOx(x＝0.8至1.2)之铌低价氧化物粉末而制得的电极的电容器。在EP 1 388 870 A1中所述的铌低价氧化物粉末尤其以0.5至2.5g/ml的流出密度为特征，而由此而制得的烧结体，则以特定的孔隙度为特征。此铌低价氧化物粉末可含有众多的其它元素，如Mg、Ca、Sr、Ba、Sc、Y、La、Ce、Pr、Ti、Zr、Hf、V、Ta、Mo、W、Mn、Re、Ru、Os、Rh、Ir、Pd、Al、C、Si以及无数的其它元素；这些元素可以50至200,000ppm的量加入，即最高达至20重量％。EP 1 388 870 A1未公开某些属于上述一组元素的存在是否有特别的好处以及特定的元素应以什么量存在。
电容器的一个重要品质特性是漏电流，即五氧化物绝缘层的剩余电流磁导率，它应尽可能低以避免损耗。杂质如Fe、Cr、Li、碱金属、卤素、碳等对剩余电流尤其有有害的影响。在基于铌低价氧化物的电容器中，这些杂质即使浓度极低仍会明显地对剩余电流产生有害的影响。如果借助标准冶金法来制备铌低价氧化物，那么就要在提高的温度于非氧化的而最好为还原的气氛中，以金属铌处理高度氧化的铌(Nb2O5)，以便平衡氧的浓度。在氧扩散进入初始金属颗粒的过程中，较小原子半径的金属杂质显然积集在该颗粒的表面层上，因为它们进行所要求的位置交换反应比铌原子更快。在阳极结构形成后，它们于是可作为缺陷获得，尤其在绝缘层之中。但是，杂质迁移至表面并非对称，而宁可说是易变的，例如取决于此任意的邻近颗粒是否恰好为该氧交换中的氧给与或氧接受颗粒。这样便引致与剩余电流峰值增加有关的杂质浓度的波动。
本发明的目的之一是降低基于铌低价氧化物阳极之电容器中的剩余电流。
本发明又一目的是减少成批制造电容器所引起的剩余电流波动。
本发明再一个目的是提供铌低价氧化物粉末，就供电容器制造的初级和次级构件而论它是有利的。
现已发现，通过以镁、钨及/或钼掺杂铌低价氧化物，对由此按照上述特性制得之电容器的剩余电流可能有有利的影响。加入晶格中的掺杂元素显然形成破坏性杂质的陷阱，即在于铌低价氧化物晶格结构中形成缺陷之掺杂元素的周围，杂质能以这样一种方式结合，使得它们对剩余电流的影响被抵消，例如根据上面提出的假设不在颗粒的表面上积集。
本发明涉及铌低价氧化物粉末，含有100至600ppm镁及/或50至400ppm钼及/或钨。以含有100至600ppm镁和50至400ppm钼及/或钨的铌低价氧化物粉末为优选。
镁的含量尤其优选地为150至400ppm，而钼及/或钨的含量尤其优选地为60至250ppm。钼优于钨，特别是同镁结合。
合适的铌低价氧化物是分子式NbOx的氧化物，式中x在0.7和1.3之间，按重量计相当于氧含量在10.8和18.3％之间；x在1和1.033之间，相当于按重量计氧含量为14.7至15.1％是可取的。尤以稍高于x＝1化学计量组成的氧含量为优选。
除了标准掺杂物如氮和磷之外，另外的杂质含量应尽可能低。钽含量或合金成分是无害的，如果它们按照分子式(Nb、Ta)Ox代替铌。特别优选的铌低价氧化物粉末，在所有情况下，具有小于15ppm的Fe、Cr、Ni、Cu、碱金属以及氟化物和氯化物含量。此外，这些含量的总和最好小于35ppm。本发明铌低价氧化物粉末的碳含量优选地应小于40ppm。
氮含量为10至500ppm是有利的。
在本发明铌低价氧化物粉末中磷含量一般是有害的。在铌和钽金属粉末中，磷用来降低次级构件和阳极构件制造过程中的烧结活度。但是在大多数情况下，通常不希望降低本发明粉末的烧结活度。根据本发明，以小于10ppm磷含量为宜。如适当在阳极构件烧结前此粉末可以磷酸、磷酸氢铵或磷酸铵加以处理。
而且，尽管不太重要的杂质，包括Al、B、Ca、Mn和Ti，优选地为小于10ppm，并且最好Si的含量不到20ppm。
本发明铌低价氧化物粉末，优选地包括烧结的初级颗粒，具有0.3至1.5μm的平均截面尺寸，尤其优选地为在0.4和1μm之间。此初级颗粒可呈小珠、薄片、细丝或其它形状。重要的是最小截面尺寸(如果形状不是圆的)处在0.3和1.5μm的范围内。
此初级颗粒烧结块最好具有按照ASTM B822(“Mastersizer”，湿润剂Daxad 11)所确定的颗粒粒度分布，它借助50至100μm的D10值、150至200μm的D50值和250至350μm的D90值明确表示。此海绵状烧结块具有圆至椭圆截面以及小于60秒/25g的好的流动特性(根据Hall，ASTM B 213)。其整体密度(根据Scoff，ASTM B 329)在0.9和1.2g/cm3(14.8至19.7g/inch3)之间。其比表面积(BET，ASTM D 3663)在0.85和2.5m2/g之间，尤其优选地在1和1.5m2/g之间。
图1给出这类包括烧结球形初级颗粒之优选粉末的SEM成像。
优选铌低价氧化物粉末极好的压制和烧结特性，也来自其烧结跨接的稳定性，它们可在烧结过程中借助温度来建立。这样的一种办法是使烧结块于超声浴中处理后改变颗粒粒度的分布。在把优选的烧结块于超声浴中处理15分钟后，一种双峰颗粒粒度分布便形成，一方面在2和10μm之间有一明显的频率最大值(副最大值)，而另一方面则在90和200μm之间(主最大值)。D10值(Mastersizer，ASTM B822)在1.5和3.0μm之间，D50值在20和60μm之间以及D90值在70和130μm之间。
本发明的优选粉末，借助汞注入确定，具有按体积为50至65％的孔隙度，尤其优选地为53至60体积％。大于90％的孔隙体积由直径在0.2和3μm之间的孔隙构成。相对于孔隙直径绘制的宽孔隙体积分布曲线有陡的侧面，在两倍于初级颗粒直径区内有一最小值。
图2给出图1所示粉末的这类孔隙大小分布曲线，孔隙亏损在1.1至1.2μm的范围。
本发明优选铌低价氧化物粉末允许使用标准方法来制备剩余电流小于0.2nA/μFV的电容器。可使剩余电流达到低至0.03nA/μFV。
因此，本发明还涉及具有铌低价氧化物阳极和铌五氧化物绝缘层的电容器，它们有小于0.2nA/μFV的剩余电流，铌低价氧化物掺杂有镁、钼及/或钨。本发明电容器的优选特性相当于上述铌低价氧化物粉末的优选特性。
本发明电容器有50,000至200,000μFV/g的比电容，优选地为70,000至150,000μFV/g。
此电容器可制备如下：
围绕插入压模中的铌或钽丝、将粉末压实至2.3至3.5g/cm3的压实密度，以形成粉末预型。得到有很好压制强度的模压件。例如，对使用301mg称入量铌低价氧化物粉末的直径5.2mm和高5.2mm圆筒形模压件(没有连接丝)，在压实至2.8g/cm3密度后所进行的标准化测量结果在施加0.5至1kg重量下是稳定的。
然后，最好于铌或钽舟中在10-8bar高真空下，在1100至1500℃使含有连接丝的模压件烧结，维持烧结时间15至25分钟，优选地约为20分钟。烧结温度按这样一种方式加以选择，使得此电容器的表面积仍为对该粉末所测得之比表面积的65至45％，它可其后由电容加以计算。最佳烧结温度和烧结维持时间，可通过烧结上述模压件以确定其压制强度而求出。烧结温度和时间最好用这样一种方式来选择，以使这种模压件能够经受8至18kg的施加负荷。
在现在的公开内容里，剩余电流和电容用下列的方法来测定：
于包括0.1重量％浓度H3PO4的电解质水溶液中，在85℃和高达30V形成电压的150mA/g形成电流以及经过愈120分钟的最终形成时间(实际上无电流)，形成烧结阳极装置。
通过将电容器浸入包括18重量％浓度H2SO4的电解质水溶液中，在温度25℃和70％形成电压的AC电压(21V)及120Hz，附加偏压10V，在3分钟的充电时间后测量其电容和剩余电流。
本发明粉末可使用标准方法来生产。标准冶金反应和合金化加工是优选的，据此，如同现在的情况，平均氧化物含量由将高度氧化产物母体或非氧化产物母体暴露于非氧化、最好为还原的气氛中，达到氧浓度平衡出现的温度来确定。除了这种固态扩散法外的方法是可以想像的，不过它们要求监控操作，从技术角度看这些以可接受的成本几乎难于对付。因此，根据本发明，最好利用高纯度可从商业途径得到的铌五氧化物，并按化学计量使之同高纯度铌金属混合，两者均呈粉末态，接着在800至1600℃的温度，于H2气氛中处理若干小时。最好此五氧化物和金属具有初级颗粒粒度，它们在氧平衡后相当于所希望的低于或稍高于1μm(最小值)截面尺寸的初级颗粒粒度。
根据本发明，最晚在氧化物成分和金属成分间的氧交换之前或过程中，尤其优选地为之前，以镁、钼及/或钨来进行掺杂是可取的。
为避免污染，所有反应器和容器，诸如坩埚、舟、筛条、网眼等，它们在升高的温度与铌或铌氧化物接触，优选由铌或钽制成，或优选衬以铌或钽。
同铌五氧化物氧交换所要求的铌金属，最好通过还原高纯度铌五氧化物以形成金属来制得。这可借助燃烧Nb2O5/Al混合物并洗去形成的铝氧化物由铝加热方法实现，然后用电子束纯化该铌金属锭。在还原和电子束熔炼后所得到的铌金属，可按已知的方法使用氢来脆化并磨细，产生薄片状的粉末。既然是这样，通过把掺杂金属加入该熔融料中掺杂就能便利地进行。
制造铌金属的优选方法遵循WO 00/67936A1的公开内容。根据这一优选的两级方法，首先在1000至1600℃，最好为高于1400℃，用氢使高纯度铌五氧化物粉末还原，以形成约有分子式NbO2的铌二氧化物，然后在900至1100℃用镁蒸气来还原至金属。用酸将此过程中形成的镁氧化物洗去。为了与本发明相一致的充分的镁掺杂，根据WO00/67936A1所述，省去最后的酸洗通常便足够。但是，在氧交换反应之前，优选地将MgO加至该金属成分及/或氧化物成分中是可取的。对于钼及/或钨掺杂，在还原该五氧化物以形成金属之前，可方便地在钼酸及/或钨酸溶液中进行浸渍。本领域的技术人员将容易熟悉另外的掺杂选择。例如，可把MoO3及/和WO3粉末加至铌五氧化物粉末或铌二氧化物粉末。以Mg和以Mo/W的掺杂，或者以Mg和Mo及/或W的优选混合掺杂，Mo优于W，尤其优选地早在制备铌五氧化物过程中便进行，例如通过把相应的掺杂物，最好为氧化物，加至Nb(OH)5，它借助用一种本身已知的方法加热而转化为铌五氧化物。
实施例1至9
起始材料为铌五氧化物粉末，通过煅烧自H2NbF7溶液中用氨水溶液沉淀所获得之铌氢氧化物来制备。其化学分析如下：
Al    ＜1ppm      As    ＜1ppm
Ca    ＜1ppm      Cl    ＜3ppm
Co    ＜0,1ppm    Cr    ＜0.3ppm
Cu    0.4ppm      F     51ppm
Fe    ＜1ppm      K     ＜0.5ppm
Mg    ＜1ppm      Mo    ＜0.3ppm
Na    2ppm        Ni    ＜0.2ppm
Si    8ppm        Ta    ＜10ppm
Ti    ＜1ppm      V     ＜1ppm
W     ＜0.5ppm    Zr    ＜0.5ppm.
此处，“＜”符号用于分析值，浓度读数在所有情况下均表示分析方法的检测限度，或者基于分析精确度可把含量表示为低于检测限度。
粉末烧结块包括烧结很均匀的圆形初级颗粒，有0.6μm的平均直径。
BET比表面积是2.4m2/g。97.5重量％烧结块小于300μm(筛分分析)。
在所有情况下，通过加入MgO粉末、MoO3粉末及/或WO3粉末使一定量该粉末同下面表1中所给出之数量(ppm)Mg、Mo及/或W掺杂，接着再在空气中煅烧。
表1：
Figure C20041006989900101
首先，在氢气氛下在1380℃通过煅烧使每种粉末1至9的一部分还原以形成NbO2。然后将此NbO2放在铌丝筛孔上，在它下面的由铌金属制成的容器中是约1.4倍化学计量的镁小片，基于NbO2的氧含量。接着在约1050毫巴压力下，在氩气氛中加热至970℃。6个小时后，在所有情况下，通过逐渐引入空气使温度慢慢冷却，以达钝化的目的。
在通过有300μm宽度筛孔的筛子筛分后，用8重量％浓度硫酸反复沥滤该粉末，洗涤并干燥以便除去所形成的MgO。
此金属粉末的表面非常凹凸不平。视批料的不同，其比表面积为4.5至5m2/g，有仅稍小的0.45至0.55μm初级结构尺寸。
按3∶1摩尔比将每种金属粉末同起始铌五氧化物混合，以这样的量使得该混合物的组成正式相当于分子式NbO。在1050毫巴的氢气氛中，慢慢把该每种混合物加热至1400℃4个小时，使之慢慢冷却并钝化。
所得到的NbO具有表2所示的掺杂元素含量。
扫描电子显微镜所确定的此初级颗粒的直径为0.5至0.65μm。其D10值为50至70μm，D50值为170至190μm，以及D90值为270至295μm。其比表面积在1和1.15m2/g之间。
表2
  实施例   Mg   Mo   W
  ppm   ppm   ppm
  1(比较)   80   -   -
  2   350   -   -
  3   84   262   -
  4   82   -   289
  5   303   187   -
  6   310   205   -
  7   294   74   69
  8   178   53   -
  9   366   81   -
另外的杂质基本上不变。有害杂质的含量如下：
C    24ppm      Cl  ＜1ppm
Cr   2ppm      Cu  0.4ppm
F    2ppm      Fe  6ppm
K    ＜1ppm    Na  2ppm
Ni   2ppm
围绕放入压模中的钽丝，由此粉末压制出直径3.6mm和长度同样3.6mm的阳极，在2.8g/cm3模压密度下，厚度为0.3mm，接着在高真空下在1460℃进行烧结20分钟。
于包括0.1重量％浓度磷酸的电解质中，在85℃和小于30V形成电压时的150mA/g形成电流下，制成阳极，在电流减弱后保持电压2个小时。
通过上述制备并配有铌五氧化物绝缘层之阳极体的电容和剩余电流，借助由18重量％浓度硫酸在25℃所模拟的对电极来测量。测量在电压21V(70％形成电压)、频率120Hz和偏压10V充电3分钟后进行。测量结果编制于表3。
表3
Figure C20041006989900121

Claims (13)

1.含有100至600ppm镁的铌低价氧化物粉末。
2.含有50至400ppm钼的铌低价氧化物粉末。
3.含有100至600ppm镁和50至400ppm钼及/或钨的铌低价氧化物粉末。
4.权利要求1至3之任一项的铌低价氧化物粉末，其中镁含量为150至400ppm。
5.权利要求1至3之任一项的铌低价氧化物粉末，其中钼含量为60至250ppm。
6.权利要求1至3之任一项的铌低价氧化物粉末，其中Fe、Cr、Ni、Cu、碱金属以及氟化物和氯化物含量在所有情况下都小于15ppm。
7.权利要求1至3之任一项的铌低价氧化物粉末，其中Fe、Cr、Ni、Cu、碱金属以及氟化物和氯化物的总量小于35ppm。
8.权利要求1至3之任一项的铌低价氧化物粉末，其碳含量小于40ppm。
9.权利要求1至3之任一项的铌低价氧化物粉末，其氮含量为10至500ppm。
10.权利要求1至3之任一项的铌低价氧化物粉末，其平均组成为NbOx，此处0.7＜x＜1.3。
11.权利要求1至3之任一项的铌低价氧化物粉末，其中包括直径为0.3至1.5μm的聚结初级颗粒。
12.由权利要求1至11之任一项的粉末烧结成的铌低价氧化物阳极。
13.包括权利要求12的铌低价氧化物阳极和铌的五氧化物绝缘层的固体电解质电容器。
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JP2009120478A (ja) 2009-06-04
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BRPI0402765A (pt) 2005-05-31
US7381396B2 (en) 2008-06-03
RU2004121476A (ru) 2006-01-10
CN1576235A (zh) 2005-02-09
ZA200405532B (en) 2005-09-28
MXPA04006812A (es) 2005-04-19
US20050013765A1 (en) 2005-01-20
DE502004011120D1 (de) 2010-06-17
US7618610B2 (en) 2009-11-17
AU2004203145A1 (en) 2005-02-03
KR20050008488A (ko) 2005-01-21
AU2004203145B2 (en) 2009-10-01
TWI367262B (en) 2012-07-01
EP1498391B1 (de) 2010-05-05
JP5546124B2 (ja) 2014-07-09
RU2369563C2 (ru) 2009-10-10
CN101407338A (zh) 2009-04-15
TW200517506A (en) 2005-06-01
JP2005035885A (ja) 2005-02-10
US20080291605A1 (en) 2008-11-27
PT1498391E (pt) 2010-06-21

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