CN101679125B - 用于氧化铬形成基底上的耐高温保护涂层的材料及其制造方法和用途 - Google Patents

用于氧化铬形成基底上的耐高温保护涂层的材料及其制造方法和用途 Download PDF

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CN101679125B
CN101679125B CN2008800118241A CN200880011824A CN101679125B CN 101679125 B CN101679125 B CN 101679125B CN 2008800118241 A CN2008800118241 A CN 2008800118241A CN 200880011824 A CN200880011824 A CN 200880011824A CN 101679125 B CN101679125 B CN 101679125B
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chromium
spinel
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米哈尔斯·库斯内佐夫
维克塔尔·绍苏克
尼克莱·托菲门克
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Abstract

本发明涉及一种用于在氧化铬形成基底上形成耐高温保护层的材料，涉及所述材料的制造方法，并且涉及所述材料的用途。所述材料适合作为在高温度下含铬合金的铬蒸发保护层(Chromverdampfungsschutzschicht)。本发明的目的是提供一种用作耐高温的、氧化铬形成合金的保护层的材料，所述材料在热和机械方面持久稳定并且在燃料电池的工作温度下保证高电导率。根据本发明，所述材料由尖晶石相和氧化二次相形成，所述氧化二次相优选是利用含锰的氧化物形成。

Description

用于氧化铬形成基底上的耐高温保护涂层的材料及其制造方法和用途
背景技术
本发明涉及用于在氧化铬形成基底上形成耐高温保护层的材料，并且涉及所述材料的制造方法及其用途。该材料适合在高温环境中用作含铬金属合金的铬蒸发保护层。
根据本发明的材料特别有利地适用于高温燃料电池。如上所述，该材料能够用于范围在550℃与1000℃之间的高温。
背景技术
使用高温燃料电池可以将化学能量直接转换成电能。
这里，阴极/电解质/阳极单元是燃料电池的核心功能元件并且包括两个电极(阴极和阳极)，这两个电极通过氧传导电解质彼此分离。
为了获得对于工业应用可接受的电压电平，需要将各电池串联连接在一起。在平面构思中，在这些不同电池之间需要安装所谓的互连接器或双极板，由此，气体馈入电极并实现各电池之间的接触。
在高温下，需要双极板的导电性尽可能好并且尽可能抗氧化。此外，金属互连接器的热膨胀系数应当相对较小，以保证与燃料电池的其它部件具有良好的热机械兼容性。
鉴于诸多限制，仅有非常少的材料可以考虑用于制造互连接器。因此首先考虑互连接器材料，在用于平面高温燃料电池时更是如此，这些平面高温燃料电池具有较高的铬含量；这些互连接器材料例如是铬基合金或铁素体钢(铁基含铬合金)。
但是，这些材料带来的问题在于：在存在氧化环境的情况下，工作温度升高时，在互连接器表面上形成三价铬氧化物层(Cr2O3)(chromium(III)oxide layer)。
氧化铬在高温下与氧和水蒸气反应，同时形成三氧化铬CrO3和氧化铬氢氧化物CrO2(OH)2/CrO(OH)4。这些新形成的含铬化合物在燃料电池的工作温度下具有高蒸气压，因此能够容易地进入到阴极中。这些含铬(Cr)物质在阴极与阴极材料反应，导致阴极材料成分发生变化，并且从长远来看，引起阴极的催化活性退化。这构成燃料电池性能降低的重要因素。
现有技术中已知有不同的材料和方法用于防止铬蒸发或者使铬蒸发最小化。这里，互连接器表面覆盖有所谓保护层的技术可获得最佳结果。
互连接器例如涂有含镧的材料，例如LaCrO3。含镧的化合物(例如LaCrO3)被直接施加到金属表面上作为保护层，或者，诸如La2O3、LaB6等化合物被施加作为反应层，从而它们在工作期间与氧化铬反应成为LaCrO3。该方法的缺点在于：在LaCrO3层中可能形成微裂缝，因而可能不能保证足够的保护以防止铬蒸发。
另一个变型在于互连接器涂覆有不含铬的钛酸钙层(Perowskitschicht)，其与阴极材料类似。所述钛酸钙层既用于保护也用于与阴极接触。但是，其缺点在于：在该层与互连接器之间的边界处形成新的铬化合物并且可能在那里生长，该层引起接触电阻的极大恶化，从而也引起燃料电池的恶化。
尖晶石化合物本身也适合作为用于保护层的有效材料。尖晶石保护层通过使用含有微合金元素(如锰、镍或钴)的钢来生成，所述钢可在在氧化环境下与源于基材料的铬共同构建尖晶石保护层。尖晶石化合物还可以通过施加含锰且与氧化铬反应后形成尖晶石化合物的层来形成。形成这些铬尖晶石结构确实导致铬蒸发减少。但是，这仍然不足以保证燃料电池具有较长使用寿命而不恶化，原因是铬仍然通过含铬的尖晶石层扩散。另外，六价铬氧化物(Cr(VI)oxide)和氢氧化铬物质由于其尖晶石相中的高铬部分而能够继续释放。
尽管如此，无铬的尖晶石化合物仍被用作保护层材料。因此，例如在DE 10306 647所公开的内容中，通过将含Co、Cu和/或Mn的氧化物施加到氧化铬形成基底上并加热到1000℃，在该基底的表面上形成成分为Co3-x-yCuxMnyO4的不透气的、不含铬的尖晶石层，其中，0＜x＜1.5，0＜y＜3并且(x+y)＜3。
例如还公开了不透气层由包含选自由锰、镁和钒组成的组的元素和选自由钴、镍、铁、铜和钒组成的组的另一元素的尖晶石层形成，形成在氧化铬形成基底上的所述不透气层即使在高达1000℃的温度下也会防止铬从该基底蒸发。
在DE 10 2005 015 755A1中公开了，在氧化工作条件下，在600℃与1000℃之间的温度下，在铬或铬化铁(FeCr)基底上涂覆氧化铬形成合金导致形成薄的、无铬的、不透气的、具有良好电导率的含氧化物尖晶石层，其中，所述铬或铬化铁基底含有浓度小于5％(重量百分比)的其他金属合金(例如锰或镁)以及选自钴、铜、铁、镍、锌、钛、锡和钒的至少两种金属。CoxCuyMn3-x-yO4、NixCuyMn3-x-yO4、CoxFeyMn3-x-yO4、FexCuyMn3-x-yO4称为可能的尖晶石层，其中，0≤x≤2，0≤y≤1并且(x+y)＜3。
但是，用于基于基底材料的一种或多种组分形成保护层的反应存在的缺点在于这些反应改变基底材料的组成。
此外，还公开了(见Journal of the Electrochemical Society 154-4(2007)，第A295-A306页)锰也能够从互连接器的阳极侧强烈蒸发。这可能导致快速消耗互连接器材料中的尖晶石形成材料，使得在表面上出现的保护层不够均匀且不够厚，不足以可靠且持续地防止铬蒸发。
在除了尖晶石化合物之外，缺少一个组成成分往往还引发形成外相。它们还引起化合物的机械强度降低，从而在所述层中特别在热负荷下引起不可修复的裂缝。这导致铬蒸发增加，并且最终导致燃料电池在持久工作方面退化。
而且，往往难以使保护层材料的热膨胀系数与金属合金的热膨胀系数相互之间精确匹配。从而在燃料电池的热循环中引起保护层裂缝，其使得该层的紧密性恶化。
在该领域中所有发明的方法均包括实现尽可能不透气的、具有匹配的热膨胀系数以及良好的电导率的保护层。但是，实现不透气的保护层在技术上非常苛刻并且通常成本高。
发明内容
因此，本发明的目的是提供一种施加作为耐高温的氧化铬形成合金的保护层的材料，所述材料在热方面和机械方面持久稳定并且在燃料电池的工作温度下保证高电导率。
这里，通过稍微改变关于热膨胀系数的成分，该材料的热膨胀系数可定位在互连接器所需的理想范围(TECRT..1000℃＝9.8-12.4ppm/K)内。而且，该材料应能够对于气相的铬物质施加收气作用(Gaetterwirkung)，由此使得在保护层的低透气性情况下也能够保证保护效果。
该目的通过权利要求1中关于所述材料的特征来实现。该材料能够通过使用根据权利要求9所述的方法来制造，并且在权利要求17中记载了适当的用途。
本发明的有利的实施例和其他演变能够通过使用在属权利要求中描述的特征来实现。
因此，根据本发明提出了一种氧化物陶瓷烧结材料，该材料是由尖晶石相(Spinellphase)和二次相(Nebenphase)形成，其中，尖晶石相优选是由镍-铜-锰/铁化合物形成，而二次相由氧化物、优选是由锰氧化物形成。
基于具有尖晶石结构的镍-铜-锰/铁化合物的本发明材料所用的相达到足够高的电导率，在上述高温下也能够保持该电导率(图2)。由于高电导率的原因，所述材料能够同时用作高温燃料电池的阴极/电解质/阳极单元的阴极表面的接触层。因此，所述材料在850℃温度下(即，在高温燃料电池的工作温度范围内)应达到至少10S/cm、优选为至少80S/cm的电导率。
在考虑到用于互连接器的材料的热膨胀系数的情况下，这也适用于热膨胀系数。这保证在主要的热条件下与互连接器材料有关的结构具有足够高的机械稳定性。
而且，基于锰氧化物的二次相具有与释放的含铬的氧化物在所述高温和存在的氧化工作气氛下反应的特性，由此，其保证了对易挥发的铬物质的附加保护。因此，能够有效地防止铬升华到阴极，以及防止阴极或阴极/电解质界面被铬污染。
基于锰氧化物的二次相的另一优点在于：它能够用作金属合金所需组分(Mn)的源。在互连接器的阳极侧由于锰蒸发而可能出现锰损耗。在该过程的工作温度下，从阴极侧到阳极侧的锰扩散可以被明显地最小化。
二次相在根据本发明的材料中只占一小部分。在持续工作中，二次相与含铬氧化物之间的反应不会对该材料的电特性和机械特性有任何实质影响。
根据本发明的材料可以在含空气的环境中或在氧气中的热处理中，通过固体反应，例如根据或使用氧化铜(二价)(CuO)、氧化镍(二价)(NiO)和氧化锰(三价)(Mn2O3)/氧化铁(三价)(Fe2O3)形成。在这里，它们将作为粉末使用。
这里，CuO在所述粉末混合物中所含部分为0-100mol.％，NiO为0-100mol.％，Fe2O3为0-100mol.％，并且Mn2O3为0-100mol.％。优选的是，Mn2O3部分应当在1-100mol.％范围内。
例如，还可以通过热注射或者通过真空涂覆工艺来施加到基底上。最后，可以例如通过本身已公开的PVD或CVD技术进行。这里，可以由粉末制成适当的目标，因而可以以这种方式涂覆。
所述氧化物的相应部分应例如在行星式球磨机中通过细致的持久搅拌/均匀化而被进行预处理。
这里，在制造过程中需要观察是否在预处理中出现其他媒介。惊人地发现，通过将乙醇混入所述粉末中，根据CuO与NiO的比例，能够获得单相或二相材料。通过额外使用酒精/乙醇能够增加第二相(二次相)的比例。
固体反应在800℃温度下已能够开始，而粉末组分的烧结在至少1000℃的温度进行。在制造过程中，维持限定的煅烧温度很重要，因为在较低的温度(＜1000℃)和较高的温度(＞1200℃)下合成的材料是多相的，由此在热和机械方面不稳定。已经表明，特别有利的是在1100℃±10℃下进行合成。
相对于化学计量式(CuO)x(NiO)y(Mn2O3)z(Fe2O3)1-z，初始化合物(Ausgangsverbindung)的摩尔比优选是为：对于铜为0.0-1.0(CuO)x，对于镍为0.0-1.0(NiO)y，对于锰为0.0-1.0(Mn2O3)，并且对于铁为0.0-1.0。
下面将参照实施方式更加具体地描述本发明。
实施方式1：
制造具有2.0mol.％以下的二次相部分的化合物：
将与组分比例(CuO)0.6(NiO)0.4(Mn2O3)对应的2.0268g CuO、1.2688g NiO和6.7044g Mn2O3称重后加入行星式球磨机中并在该行星式球磨机中均匀化24小时以上。均匀的粉末经过筛虑并且在1100℃温度下烧结15小时。
这样制造出的材料具有尖晶石相Cu0.6Ni0.4Mn2O4成分。这里，二次相(MnOx)1-y+(CuO/NiO)y(1＜x1.5且0＜y＜0.5)部分在2.0mol.％以下。
实施方式2：
制造具有2.0-5.0mol.％的二次相部分的化合物：
将与组分比例(CuO)0.6(NiO)0.4(Mn2O3)对应的2.0268g CuO、1.2688g NiO和6.7044g Mn2O3称重后加入行星式球磨机中并添加10ml乙醇，并且在该行星式球磨机中均匀化24小时以上。均匀的粉末在70℃温度下干燥，然后经过筛虑。经过筛虑的粉末在1100℃温度下烧结15小时。
这样制造出的材料具有尖晶石相Cu0.6Ni0.4Mn2O4成分。这里，二次相(MnOx)1-y+(CuO/NiO)y(1＜x1.5且0＜y＜0.5)部分达到2.0和5.0mol.％。
实施方式3：
为了制造具有2.0mol.％以下的二次相部分的化合物，将2.6893g CuO、0.6313g NiO和6.3382g Mn2O3和0.6748g Fe2O称重后加入，以获得(CuO)0.8(NiO)0.2(Mn2O3)0.95(Fe2O3)0.1的组分比例。向该混合物添加10ml乙醇并且在行星式球磨机中均匀化24小时以上。随后在70℃温度下进行干燥。然后经过筛虑的粉末在1100℃温度下进行15小时以上的热处理。这样获得的材料具有尖晶石相Cu0.8Ni0.2Mn0.9Fe0.1O4成分。这里，二次相(MnOx)1-y+(CuO/NiO)y(1＜x1.5且0＜y＜0.5)部分在2.0mol.％以下。
附图说明
图1是根据本发明合成的材料的X射线衍射图；
图2是示出不同化合物的温度相关的电导率的示图；
图3是示出关于合金钢Crofer22APU和Ducrolloy合金(Ducrolloy-Legierung)的、温度与材料热膨胀系数的关系的示图；
图4a示出按照抛光模式(Schliffbild)的层设计；以及
图4b示出热处理后在Crofer22APU基底上的层系的EDX频谱。
具体实施方式
利用图1所示的X衍射图，可见在1100℃下烧结的材料的相成分(Phasenzusammensetzung)取决于制造过程。图1和图2与利用化学计量(CuO)0.6(NiO)0.4(Mn2O3)分别根据实施方式1和实施方式2制造的化合物对应。
在根据图2的示图中关于具有不同CuO/NiO比例的化合物(CuO)x(NiO)y(Mn2O3)示出温度与电导率的关系。
从图3所示示图中，关于特种钢Crofer22APU和Ducrolloy合金在0℃至900℃的温度范围内示出具有不同CuO/NiO比例的(CuO)x(NiO)y(Mn2O3)的热膨胀系数，并明显可见，在工作温度这些材料的热膨胀系数仅有细微差别，从而它们能够相互结合使用，即使与高温燃料电池结合也不存在问题。
图4a示出在空气中850℃下进行100小时热处理后，在涂覆有保护层的基底上形成的层系的典型结构。根据实施方式1的材料通过滚涂被施加到基底Crofer22APU上。O、Cr、Mn、Fe、Cu、Ni的相关EDX元素轮廓(图4b)清楚地示出该层结构。
在基底(区域1)与保护层之间的边界处形成了薄的铬/锰混合氧化物层(区域2)。包含根据本发明的材料的外层(区域3)不包含通过EDX可检测到的铬部分。
用于含铬保护层的根据本发明的材料由于其化学特性、热特性和电特性，所以能够用于高温燃料电池中。

Claims (5)

1.一种用于氧化铬形成基底上的耐高温保护层的材料，所述材料包含尖晶石相和氧化第二相，其中，
所述尖晶石相具有组成(CuxNi1-x)y(Mn1-zFez)2O4，其中0＜x＜1.0，0.8≤y≤1.2且0.0＜z＜1.0，以及所述第二相具有组成(MnOx)1-y+(CuO/NiO)y，其中1<x<1.5且0<y<0.5。
2.根据权利要求1所述的材料，其特征在于，以0.1-20Vol.%的比例包含所述第二相。
3.根据权利要求1所述的材料，其特征在于，所述第二相均匀分布在所述尖晶石相中。
4.根据权利要求1所述的材料，其特征在于，所述材料在850℃下具有至少10S/cm的电导率。
5.根据权利要求1至4之一所述的材料用于制造保护层和用于高温燃料电池的阴极-电解质-阳极单元的阴极的电接触的用途。
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