CN102603002A - 部分还原铌金属氧化物的方法和脱氧的铌氧化物 - Google Patents

部分还原铌金属氧化物的方法和脱氧的铌氧化物 Download PDF

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CN102603002A
CN102603002A CN2012100630011A CN201210063001A CN102603002A CN 102603002 A CN102603002 A CN 102603002A CN 2012100630011 A CN2012100630011 A CN 2012100630011A CN 201210063001 A CN201210063001 A CN 201210063001A CN 102603002 A CN102603002 A CN 102603002A
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niobium oxide
niobium
getter material
deoxidation
oxide
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詹姆斯.A.法伊夫
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Cabot Corp
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Abstract

本发明所描述的是至少部分地还原铌氧化物的方法，其中该方法包括在消气材料(getter material)存在下对铌氧化物进行热处理，该热处理是在允许氧原子从起始的铌氧化物转移至消气材料的气氛中进行的，并且在足够的温度下进行足够的时间，以形成脱氧的铌氧化物。本发明也描述了铌的氧化物和/或低价氧化物，还描述了包含由该铌氧化物和低价氧化物制成的阳极的电容器。

Description

部分还原铌金属氧化物的方法和脱氧的铌氧化物
本申请是中国发明申请(发明名称：部分还原铌金属氧化物的方法和脱氧的铌氧化物，申请日：1999年9月15日；申请号：99811568.1)的分案申请。
发明背景
本发明涉及铌及其氧化物，更具体地涉及铌氧化物和至少部分还原铌氧化物的方法，并且进一步涉及脱氧的铌。
发明概述
依据本发明的目的，如这里所概括和描述的那样，本发明涉及至少部分还原铌氧化物的方法，该方法包括在消气材料的存在下，于允许氧原子从铌氧化物转移至消气材料(getter material)的气氛中，对铌氧化物进行足够温度与时间的热处理，以形成脱氧的铌氧化物。
本发明还涉及脱氧的铌氧化物，该脱氧的铌氧化物优选具有有益的特性，尤其是在形成电解电容器阳极时。例如，由本发明的脱氧铌氧化物制成的电容器，可以具有相当于约200000CV/g或更高的电容量。另外，由本发明的脱氧铌氧化物制成的电解电容器阳极具有低的直流(DC)漏电。例如，这种电容器可以具有从约0.5nA/CV至约5.0nA/CV的直流漏电。
因此，本发明还涉及增加电容量和降低由铌氧化物制成的电容器中直流漏电的方法，该方法包括部分地还原铌氧化物，所述的还原是通过在消气材料的存在下，于允许氧原子从铌氧化物转移至消气材料的气氛中，热处理铌氧化物而进行的，并且在足够的温度下进行足够的时间，以形成脱氧的铌氧化物，该脱氧的铌氧化物在形成电容器阳极时，降低直流漏电和/或增加电容量。
应当理解，无论是前面的概述还是下面的详述都仅仅是示范性和说明性的，其目的是进一步解释本发明。
附图简述
图1-11是本发明的铌氧化物于各种放大倍数下的扫描电子显微图。
发明详述
在本发明的一个实施方案中，涉及至少部分还原铌氧化物的方法。一般地，该方法包括在消气材料存在下，于允许氧原子从铌氧化物转移至消气材料的气氛中，对铌氧化物原料进行足够时间与温度的热处理，以形成脱氧的铌氧化物的步骤。
为了本发明的目的，铌氧化物可以是至少一种铌金属和/或其合金的氧化物。铌氧化物原料的具体实例是Nb2O5。
本发明所使用的铌氧化物可以是任何形状或任何尺寸的。优选地，该铌氧化物为粉末状或各种颗粒状。可以使用的粉末类型包括，但不限于，片状的、角状的、球状的、以及它们的混合物或变种。该铌氧化物优选为更有效地产生脱氧铌氧化物的粉末状。
这种优选铌氧化物粉末的实例，包括那些网目尺寸从约60/100至约100/325目和从约60/100至约200/325目的铌氧化物粉末。另一尺寸范围是从-40目至约-325目。换言之，优选的铌氧化物粉末具有约150/250至约45/150微米和约150/250至约45/75微米的粒度，另一优选的尺寸范围是约355微米至约45微米。
用于本发明的消气材料，是任何能够将特定铌氧化物原料还原为脱氧铌氧化物的材料。优选的消气材料包括钽、铌、或二者都包括。其他实例包括，但不限于，镁等。可以使用任何对氧的亲和力大于铌氧化物的消气材料。更优选的消气材料是铌。本发明的铌消气材料，是含有可以至少部分地消除或还原铌氧化物中的氧的任何材料。这样，铌消气材料可以是合金，也可以是包含铌金属与其他成分的混合物的材料。优选的铌消气材料，如果不是专门地，主要地为铌金属。铌消气材料的纯度不是重要的，但还是优选包含高纯铌的消气材料，以避免在热处理期间引入其他杂质。因此，铌消气材料中的铌金属优选具有至少约98％的纯度，更优选具有至少约99％的纯度。铌消气材料中的氧含量是任意的。优选如铁、镍、铬和碳等影响直流漏电的杂质低于约100ppm。更优选的消气材料是铌金属片，其优选具有大于约75000CV/g的高电容量，更优选具有约100000CV/g或更高如200000CV/g的电容量。所述的消气材料还优选具有高表面积，如BET为约5至约30m2/g，更优选为约20至约30m2/g。所述的消气材料包含氢化钽颗粒，并可以是14/40目的氢化钽颗粒。
消气材料可以是任何形状或尺寸。例如，可以是浅盘状，其中包含要还原的铌氧化物，也可以是颗粒或粉末尺寸的。消气材料优选为粉末状，以便具有还原铌氧化物最有效的表面积。这样，消气材料可以是片状的、角状的、球状的、以及它们的混合物或变种，例如粗糙的碎片，如通过筛
分可容易从粉末产品中分离出来的14/40目碎片。
类似地，消气材料也可以是碳等，并且可以具有与上述铌消气材料相同的优选参数和/或性能。其他消气材料可以单独使用，也可以与钽或铌消气材料组合起来使用。此外，消气材料可以部分地包含其他的材料。
消气材料使用之后可以除去，也可以保留下来。优选地，如果消气材料与脱氧的铌氧化物保留下来，那么该消气材料优选为铌，且优选具有与铌氧化物原料相似的形状和尺寸。而且，优选使用高纯度、高表面积和/或高多孔性消气材料(如电容器级材料)，因为这样的材料会得到与脱氧的铌氧化物相同或相似的氧化状态，从而使本方法取得100％的脱氧铌氧化物产量。因此，消气材料可以作为消气材料，也可以保留下来而成为脱氧的铌氧化物的一部分。
一般地，存在足够量的消气材料，以至少部分地还原热处理中的铌氧化物。进一步讲，消气材料的量取决于所需要的对铌氧化物的还原量。例如，如果需要轻度地还原铌氧化物，那么消气材料将按化学计量量加入。类似地，如果铌氧化物需要就其所存在的氧充分地还原，那么消气材料应按2至5倍的化学计量量加入。通常，消气材料的加入量(如按钽消气材料计，为100％的钽)，按消气材料与存在的铌氧化物的量的比例，可以从约2∶1至约10∶1。消气材料优选在允许氧原子从铌氧化物转移至消气材料的气氛(如氢气气氛)中，与铌氧化物原料共混或混合在一起，并且优选在约1100至1500℃的温度下混合。
而且，消气材料的量也可以依据要还原的铌氧化物的类型而定。例如，当要还原的铌氧化物为Nb2O5时，消气材料的量优选为5∶1。另外，由Nb2O5开始时，使用化学计量量的消气材料，优选铌金属片，以产生优选为0.89份金属对1份氧化物的氧化物。
铌氧化物原料所要经受的热处理，可以在如铌和钽等金属的热处理中常用的任何热处理设备或炉子中进行。在消气材料存在的情况下，铌氧化物的热处理，是在足够的温度下进行足够的时间，以形成脱氧的铌氧化物。热处理的温度和时间，可以依据多种因素如铌氧化物的还原量、消气材料量、消气材料的类型以及铌氧化物原料的类型而定。一般地，铌氧化物的热处理温度为约800℃或更低至约1900℃，更优选为约1000℃至约1400℃，最优选约1100℃至约1250℃。更具体地，所述的热处理温度为约1000℃至约1300℃，优选所述热处理在约1000℃至约1500℃的温度下进行约10至约90分钟，更优选约1100℃至约1250℃进行约5分钟至约100分钟，更优选进行约30分钟至约60分钟。鉴于本申请，常规的试验允许本领域技术人员容易地控制热处理的时间和温度，以便使铌氧化物适宜地或合乎需要地还原。
热处理在允许氧原子从铌氧化物转移至消气材料的气氛中进行。该热处理优选在含氢的气氛中进行，所述的含氢气氛最好就是氢气。其他气体如惰性气体也可以与氢一起加入，只要该其他气体不与氢反应。热处理过程中存在的氢气气氛的压力，优选为约10托至约2000托，更优选为约100托至约1000托，最优选为100托至约930托。也可以使用H2与惰性气体如Ar的混合物。此外，还可以使用N2中的H2，以实现对铌氧化物的N2含量的控制。其中所述的消气材料先于或在热处理步骤的过程中与铌氧化物均质化。
在热处理过程中，可以使用恒定的热处理温度于整个热处理过程，也可以使用变化的温度或温度阶梯。例如，氢气可以1000℃初始导入，然后用30分钟升温至1250℃，然后再降温至1000℃并保持至移除H2气体。移除H2或其他气氛之后，可以降低炉子的温度了。可以用这些阶梯的变化去适合工业上的任何优选项。随后，脱氧的铌氧化物可以通过如粉碎减小尺寸。脱氧的铌氧化物可以以处理电子管金属的任何其他方法，凝聚和粉碎或处理。
脱氧的铌氧化物也可以包含不同量的氮，如从约100ppm至约30000ppm的N2。
脱氧的铌氧化物是其中的氧含量低于铌氧化物原料的任何铌氧化物。有代表性的脱氧铌氧化物包括NbO、NbO0.7、NbO1.1、NbO2及其与或不与存在的其他氧化物的任意组合。通常，本发明的脱氧铌氧化物所具有的铌对氧的原子比为约1∶小于2.5，优选为1∶2，更优选为1∶1.1、1∶1或1∶0.7。按另一种方式，所述脱氧的铌氧化物优选具有NbxOy式，其中Nb为铌，x为2或更小，y小于2.5x。更优选x为1而y小于2如1.1、1.0、0.7等。
铌氧化物原料可以通过在1000℃煅烧直至除去任何挥发性组分来制备。该氧化物可以通过筛子来分级。可以用铌氧化物的预热处理来建立氧化物颗粒的受控孔隙度。
本发明的脱氧的铌氧化物还优选具有微孔性的表面，并且优选具有象海绵一样的结构，其中的初级颗粒优选为约1微米或更低。扫描电子显微图进一步描述本发明优选的脱氧铌氧化物的类型。从这些显微图可以看出，本发明的脱氧铌氧化物具有高的比表面积和孔隙度约50％的多孔结构。所述的铌氧化物具有约0.1至约10微米小孔的多孔结构。另外，本发明的脱氧铌氧化物可以用比表面积来表征，优选的比表面积为约0.5至约10.0m2/g，更优选为约0.5至约2.0m2/g，最优选为约1.0至约1.5m2/g。铌氧化物粉末的表观密度优选为低于约2.0g/cc，更优选为低于约1.5g/cc，最优选为低于约0.5至1.5g/cc。此外，所述的铌氧化物粉末可以具有约5g/in3至约35g/in3的Scott密度。
本发明使用较少的铌于产品中却能够获得类似于，如果不优于，铌的性能，这是因为形成并利用了脱氧的铌氧化物。因此，本发明扩大了如电容器阳极等产品中铌的数量，因为用相同数量的铌可以制造更多的阳极或其他产品。
本发明的各种脱氧铌氧化物还可以用电性能来表征，所述的电性能产生于本发明的脱氧铌氧化物所形成的电容器阳极。一般地，可以测试本发明的脱氧铌氧化物的电性能，办法是将脱氧的铌氧化物粉末压制成阳极，并在适宜的温度下烧结所压制的粉末，然后做阳极氧化处理，以制备电解电容器的阳极，随后就可以测试该阳极的电性能。
因此，本发明的另一实施方案涉及由本发明的脱氧铌氧化物制成的电容器阳极。可以按类似于制造金属阳极的方法，用粉末状的脱氧氧化物制备阳极，即压制嵌入了导线或其他连接器的多孔球团，然后进行任选的烧结和阳极氧化处理。导线连接器可以在阳极氧化之前的任何时候嵌入或贴附。用本发明的某些脱氧铌氧化物制成的阳极，可以具有约1000CV/g或更低至约300000CV/g或更高的电容量，其他范围的电容量可以从约20000CV/g至约300000CV/g，或从约62000CV/g至约200000CV/g，并优选为约60000至约150000CV/g。形成本发明的电容器阳极时，可以使用允许形成具有所需特性的电容器阳极的烧结温度。烧结温度取决于所用脱氧铌氧化物。当使用脱氧的铌氧化物时，烧结温度优选为约1200℃至约1750℃，更优选为约1200℃至约1400℃，最优选为约1250℃至约1350℃。
由本发明的铌氧化物形成的阳极，优选在35伏的电压下赋能，更优选在约6伏至约70伏的电压下赋能。当使用脱氧的铌氧化物时，赋能电压优选为约6伏至约50伏，更优选为约10伏至约40伏。也可以使用其他较高的赋能电压。脱氧的铌氧化物阳极可以按如下办法制备，即制造带有导线
的Nb2O5球团，然后于氢气气氛或其他适宜的气氛中，在如粉化氧化物的消气材料附近进行烧结。在该实施方案中，所制备的阳极产品可以直接制备，例如，同时形成脱氧的电子管金属氧化物和阳极。此外，由本发明的脱氧铌氧化物所形成的阳极，优选具有低于约5.0nA/CV的直流漏电。在本发明的一个实施方案中，由本发明的一些脱氧铌氧化物所形成的阳极，具有约5.0nA/CV至约0.50nA/CV的直流漏电。
本发明还涉及一种根据本发明的电容器，该电容器表面具有铌氧化物薄膜。所述的薄膜优选为铌的五氧化物薄膜。将金属粉末制成电容器阳极的方法对本领域的技术人员是已知的，而且这些方法，如美国专利US 4805074、5412533、5211741和5245514，以及欧洲专利申请0634762A1和0634761A1中所阐述的方法，全部整体性地引入本文作为参考。
本发明的电容器可以用于各种终端用途，如汽车用电子设备，移动电话，计算机的监视器、母板等，消费电子产品包括电视和显示器、打印机/复印机、电源、调制解调器、笔记本计算机、磁盘驱动器等。
通过下面的实施例，本发明将得到进一步的阐明，所述的实施例是用来解释本发明的。
试验方法
阳极的制造
尺寸-0.197″直径
3.5Dp
粉末重量＝341mg
阳极的烧结
1300℃    10′
1450℃    10′
1600℃    10′
1750℃    10′
30V Ef阳极氧化
30V Ef60℃/0.1％H3PO4电解质
20mA/g恒定电流
直流漏电/电容量-ESR测试：
直流漏电测试---
70％Ef(21V直流电)试验电压
60秒充电时间
10％H3PO421℃
电容量-DF测试：
18％H2SO421℃
120Hz
50V Ef再赋能阳极氧化(Reform Anodization)：
50V Ef60℃/0.1％H3PO4电解质
20mA/g恒定电流
直流漏电/电容量-ESR测试：
直流漏电测试---
70％Ef(35V直流电)试验电压
60秒充电时间
10％H3PO421℃
电容量-DF测试：
18％H2SO421℃
120Hz
75V Ef再赋能阳极氧化：
75V Ef60℃/0.1％H3PO4电解质
20mA/g恒定电流
直流漏电/电容量-ESR测试：
直流漏电测试---
70％Ef(52.5V直流电)试验电压
60秒充电时间
10％H3PO421℃
电容量-DF测试：
18％H2SO421℃
120Hz
根据美国专利US 5011742、4960471和4964906中阐述的方法，进行Scott密度、氧分析、磷分析和BET分析的测定，所有文献均整体引入本文作为参考。
实施例
实施例1
伴有约50ppm氧的+10目氢化钽碎片(99.2克)与22克Nb2O5混合，并置于钽盘中。将所述的钽盘置于真空热处理炉中并加热至1000℃。将氢气引入炉中至+3psi的压力。将温度进一步均匀地升高至1240℃并保持30分钟。在6分钟内降温至1050℃，直至全部氢气从炉中清扫干净。仍保持1050℃的同时，从炉中排除氩气至压力为5×10-4托。在该点，再次导入700mm的氩气至炉膛，并将炉子冷却至60℃。
在从炉子移出之前，令材料循环地暴露于分压逐渐升高的氧气若干次以使之钝化如下：炉子回填氩气至700mm，然后充入空气至1个大气压。4分钟后，排空炉膛至10-2托。炉膛回填氩气至600mm，然后充入空气至1个大气压并保持4分钟。排空炉膛至10-2托，然后回填氩气至400mm，再充入空气至1个大气压。4分钟后，排空炉膛至10-2托。炉膛回填氩气至200mm，然后充入空气至1个大气压并保持4分钟。排空炉膛至10-2托。用空气回填炉膛至1个大气压并保持4分钟。排空炉膛至10-2托。用氩气回填炉膛至1个大气压，并打开炉子取出样品。
通过40目的筛子筛分，将粉末产物从钽碎片消气剂中分离出来。产品的测试结果如下。
1300℃烧结10分钟并于35V下赋能的球团的CV/g＝81297
nA/CV(直流漏电)＝5.0
球团的烧结密度＝2.7g/cc
Scott密度＝0.9g/cc
化学分析(ppm)
C＝70
H2＝56
Ti＝25    Fe＝25
Mn＝10    Si＝25
Sn＝5     Ni＝5
Cr＝10    Al＝5
Mo＝25    Mg＝5
Cu＝50    B＝2
Pb＝2     其他元素＜检出限
实施例2
样品1至20是使用如表中所指出的粉末化Nb2O5，并遵循类似于上述步骤的实例。对于多数实例，原料的网目尺寸列于表中，如60/100，意思是比60目小但比100目大。类似地，给出了某些钽消气材料的筛子尺寸为14/40。标记为“氢化钽碎片”的消气材料为+40目，没有颗粒尺寸的上限。
样品18用铌作消气材料(商业上可从CPM得到N200的片状铌粉末)。样品18的消气材料是不与最终产品分离的细粒状的铌粉末。X-射线衍射表明一些消气材料仍然是铌，但大多数通过与铌氧化物原料Nb2O5一样的处理而转化成NbO1.1和NbO。
样品15是Nb2O5球团，压缩至接近固体密度，并与H2在钽消气材料附近反应。热处理使固体氧化物球团转化成多孔的NbO低价氧化物块。将该块烧结成铌金属条，以建立阳极的引线，并用类似于粉末块球团的电赋能方法，阳极氧化至35伏。该样品证实了该方法的独特能力，即以一简单的步骤从Nb2O5原料迅速地对块阳极氧化。
表中示出，由本发明的压制和烧结粉末/球团可以制备高电容量和低直流漏电的阳极。给出了各种样品的显微照片(SEM)。这些照片示出了本发明的脱氧铌氧化物的多孔结构。具体地，图1是球团外表面的5000倍照片(样品15)。图2是同样球团的内部的5000倍照片。图3和图4是相同球团的外表面的1000倍照片。图5是样品11的2000倍照片，图6和图7是样品4的5000倍照片。图8是样品3的2000倍照片，图9是样品6的3000倍照片。最后，图10是样品6的3000倍照片，图11是样品9的2000倍照片。
Figure BDA0000142486760000101
根据本发明所公开的说明书和实践，本发明的其他实施方案对本领域的技术人员将是显而易见的。说明书和实施例的目的仅是对本发明的解释，本发明的真正精神和范围见下面的权利要求书。

Claims (40)

1.一种至少部分还原铌氧化物的方法，包括在消气材料存在下，于允许氧原子从铌氧化物转移至消气材料的气氛中，对铌氧化物进行足够时间与温度的热处理，以形成脱氧的铌氧化物；其中所述铌氧化物为五氧化二铌。
2.权利要求1的方法，其中所述脱氧的铌氧化物为铌的低价氧化物。
3.权利要求1的方法，其中所述脱氧的铌氧化物所具有的铌对氧的原子比例为1∶小于2.5。
4.权利要求1的方法，其中所述脱氧的铌氧化物所具有的氧含量低于完全氧化的铌的化学计量。
5.权利要求1的方法，其中所述脱氧的铌氧化物具有微孔结构。
6.权利要求1的方法，其中所述脱氧的铌氧化物具有50％的孔隙体积。
7.权利要求1的方法，其中所述的气氛是以10托至2000托的量存在的氢气。
8.权利要求1的方法，其中所述的消气材料是形成阳极时电容量至少为75000CV/g的铌消气材料。
9.权利要求1的方法，其中所述的气氛为氢气气氛。
10.权利要求1的方法，其中所述的消气材料为形成阳极时电容量为100000CV/g至200000CV/g的铌消气材料。
11.权利要求1的方法，其中所述的热处理是在1000℃至1500℃的温度下进行10至90分钟。
12.权利要求1的方法，其中所述的消气材料先于或在热处理步骤的过程中与铌氧化物均质化。
13.权利要求1的方法，其中所述的消气材料是片状的铌消气材料。
14.权利要求1的方法，其中所述的消气材料为铌消气材料，并在热处理之后形成脱氧的铌氧化物。
15.权利要求1的方法，其中所述的消气材料是含镁的消气材料。
16.权利要求1的方法，其中所述的消气材料包含氢化钽颗粒。
17.权利要求1的方法，其中所述的消气材料包含钽、铌，或二者都包含。
18.权利要求1的方法，其中所述的消气材料是14/40目的氢化钽颗粒。
19.权利要求1的方法，其中所述的消气材料是电容器级材料。
20.一种铌氧化物，其中所述的铌氧化物包含NbO、NbO0.7、NbO1.1、或它们的组合，其比表面积为0.5～10m2/g，其中所述铌氧化物为粉末，所述的铌氧化物具有0.1至10微米微孔的多孔结构，和所述铌氧化物用于电容器阳极。
21.权利要求20的铌氧化物，具有5g/in3至35g/in3的Scott密度和/或低于2.0g/cc的表观密度。
22.权利要求20的铌氧化物，其中还包含氮。
23.权利要求30的铌氧化物，其中所述的氮以100ppm至30000ppm的N2存在。
24.一种电解电容器阳极，其是由权利要求20的铌氧化物形成的，所述阳极的电容量高达300000CV/g。
25.一种电解电容器阳极，其是由权利要求20的铌氧化物形成的，所述阳极的电容量为1000至300000CV/g。
26.权利要求25的电解电容器阳极，其中所述阳极的电容量为60000至200000CV/g。
27.权利要求25的电解电容器阳极，其具有0.5至5nA/CV的直流漏电。
28.权利要求20的铌氧化物，其中所述的铌氧化物包括球状的、片状的、角状的、或它们的组合。
29.权利要求20的铌氧化物在制备电容器中的用途。
30.权利要求25的电解电容器阳极在制备电容器中的用途。
31.一种电解电容器阳极，其是由权利要求20的铌氧化物，在1200℃至1750℃的温度下进行烧结而制备的。
32.一种电解电容器阳极，其是由权利要求20的铌氧化物，在1200℃至1450℃的温度下进行烧结而制备的。
33.权利要求29的用途，具有1000至300000CV/g的电容量。
34.权利要求29的用途，具有60000至200000CV/g的电容量。
35.权利要求29的用途，具有0.5至5nA/CV的直流漏电。
36.制备电容器阳极的方法，包括a)制造铌氧化物球团，并且在消气材料存在下，于允许氧原子从铌氧化物转移至消气材料的气氛中，对该球团进行足够时间与温度的热处理，以形成包括该球团的电极体，其中该球团包含脱氧的铌氧化物，和b)阳极氧化处理所述的电极体，以形成所述的电容器阳极，其中所述铌氧化物为五氧化二铌。
37.权利要求36的方法，其中所述的气氛是氢气气氛。
38.权利要求36的方法，其中所述的消气材料包含钽、铌，或二者都包含。
39.权利要求36的方法，其中所述的消气材料是铌。
40.权利要求36的方法，其中所述脱氧的铌氧化物具有的铌对氧的原子比例为1∶小于2.5。
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Application publication date: 20120725