CN101137864A - 隔热材料及其制备方法和用途 - Google Patents

隔热材料及其制备方法和用途 Download PDF

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CN101137864A
CN101137864A CN200680007846.1A CN200680007846A CN101137864A CN 101137864 A CN101137864 A CN 101137864A CN 200680007846 A CN200680007846 A CN 200680007846A CN 101137864 A CN101137864 A CN 101137864A
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G·普拉克特
R·瓦森
D·斯托弗
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Abstract

本发明涉及隔热材料，其特别在高于1150℃、特别是高于1200℃的高温下相稳定，并具有非常好的长时间稳定性。所述隔热材料可以以多相存在，其中至少一个相具有磁铁铅矿结构，并且按化学计量含有0.1－10mol％的M12O3、0.1－10mol％的Li2O和其余为M22O3和附带杂质，其中M1选自元素镧、钕、钆或者它们的混合物，M2选自元素铝、镓、铁或它们的混合物。对于该相特别有利的组合物为组成为LaLiAl11O18.5或者LaLi0.5Al11.5O19的相。所述隔热材料可以通过常用方法施加到高热负荷的构件上，例如涡轮机叶片。其既适合单独作为隔热层，又适合例如在材料复合物中与YSZ联用。在该隔热材料中有规律存在的断裂裂纹有助于在频繁的交替负载情况下降低隔热层和被涂覆构件之间的应力。

Description

隔热材料及其制备方法和用途
本发明涉及隔热材料，特别是在高于1150℃下使用的隔热材料，例如用于比如用于发电厂或者飞机发动机的燃气轮机的隔热材料。此外，本发明涉及制备该隔热材料的方法。
背景技术
迄今为止，作为用于在超过1000℃高温下的典型隔热层材料经证实合适的是正方晶系或者稳定化的ZrO2。其作为氧化物覆层存在于金属基材上，该基材特别由高合金Ni基材料组成。所述隔热材料直接设置在基材上，或者经额外的中间层(其用作粘附剂层)设置在基材上。为了施加陶瓷覆层，适用大气等离子体喷镀(APS)或者借助电子束蒸镀(EE-PVD)。
迄今所用的覆盖层和粘合剂层在其交替热负载承受能力、其抗氧化性及其长时间稳定性方面仍然存在一些问题。
对于基于ZrO2的覆层已知的是，其在高于1000℃温度不够稳定且其导热性增加。同时，出现多孔结构致密化。在频繁的温度交替情况下，这两种作用常常不利地导致覆层的剥落。
迄今作为标准隔热材料使用的用Y2O3部分稳定化的氧化锆(YSZ)在高于1200℃的温度下遭受相变，所述相变在冷却时可不利地导致隔热层的剥落。与位于隔热层之下的金属层(例如镍高温合金)相比，YSZ通常具有较低的热膨胀系数。这在热负载条件下导致形成裂纹。在长时间使用时，YSZ显示出显著的烧结行为，且被烧结层的E模量显著上升。由此，隔热层丧失其应力容差(Spannungstoleranz)，使得可以易于导致整个层的剥落。
此外，在高于800℃温度下，YSZ具有对于氧的良好离子传导能力。这促进了设置在隔热层和金属层之间的粘合剂层的不利的氧化。结果，该粘合剂层的热膨胀系数以同样促进隔热层剥落的方式不利地改变。
已知的是，六铝酸镧作为新的隔热材料具有直至1400℃的长时间稳定性。与基于锆的市售隔热层相比，在这种高温下六铝酸镧变化显著较慢。典型的组成优选为小片式构造，这有利地防止了在烧结期间层的致密化。这类特别合适的代表物包括La2O3、Al2O3和MgO。其中晶体结构对应于磁铁铅矿。
由DE19807163C1已知例如一种隔热材料，其热化学稳定和相稳定地有利地适用于高温应用。所述材料具有总通式M2O3-xMeO-yAl2O3，其中M＝La或者Nd，Me＝碱土金属，过渡金属或稀土，特别是Mg、Zn、Co、Mn、Fe、Ni、Cr。系数x和y具有优选范围0.2≤x≤3.3，且10.0≤y≤13。作为理想组成公开了LaMgAl11O19，其以磁铁铅矿结构结晶并具有大约7.1mol％La2O3，大约14.3mol％MgO和大约78.6％Al2O3。
任务和解决方案
本发明的任务在于，提供用于在高温下、特别在高于1150℃温度下使用的另一种隔热材料，其克服了现有技术的上述缺陷，和特别由于其应力容差而具有非常好的长期性能。
本发明的任务通过具有主权利要求的总体特征的隔热材料以及通过根据副权利要求的制备方法得以实现。此外，本发明的任务通过根据另一副权利要求的用途得以实现。所述材料的有利构造，制备和应用参见它们的各从属权利要求。
发明内容
从DE19807163C1公开的隔热材料的优良特性出发，在本发明范围内令人惊奇地发现，用锂代替在DE19807163C1中所述的碱土金属、过渡金属、稀土或它们的混合物而掺杂以这种磁铁铅矿结晶析出的相，带来了额外的惊人的积极特性。在本发明的隔热材料情况下，其涉及根据式Ml2O3-xLi2O-yM22O3的组合物。其中M1＝镧、钕或者钆或它们的混合物，而M2＝铝、镓或铁和它们的混合物。所述材料主要由M2氧化物组成，其在给定间距具有由Ml2O3和氧化锂组成的单层。替代氧化铝，特别可以使用氧化镓或者氧化铁作为M22O3。氧化镧同样可以由稀土氧化物，特别是由钕或钆替代。
Ml2O3的引入通常导致形成具有特征小片状晶体结构的层结构。优选地，形成这样的磁铁铅矿，其通常仅具有非常窄的材料组成范围。磁铁铅矿结构的典型组成MlM211O18在晶格中具有由结构引起的非常多的阳离子(大约8％M1元素)和阴离子(大约5％氧)空穴位置，其允许原子扩散通过该晶格结构。这种有利的相的典型代表物例如是LaAl11O18、LaGa11O18、LaFe11O18、NdAl11O18、NdGa11O18、NdFe11O18或者GdAl11O18、GdGa11O18、GdFe11O18。
如由DE169807163C1已知的，由于计量添加具有小离子直径的二价阳离子(例如Mg2+、Mn2+、Co2+、Zn2+等，相的均匀区域由LaAl11O18扩大到直至LaMgAl11O19。在该最优化的组合物中，化合物在其组成中几乎不再有波动宽度。另外添加La2O3和例如MgO常常导致结构中的重新缺陷和形成多相区域。
在DE169807163C1中公开的材料在最佳情况下是LaMgAl11O19，其在晶格结构中绝无结晶学缺陷。所有存在的空穴位置通过添加MgO也即Mg2+和O2-离子占据。正是这种完全的占据在高于1000℃温度范围内导致所需的高热化学稳定性和相稳定性。
与此相反，本发明的隔热材料是具有根据式M12O3-xLi2O-yM22O3的组成的化合物，其可以以多相存在，但是其中用锂掺杂的相必需存在于磁铁铅矿结构中。这意味着，替代用二价离子例如Mg2+、Mn2+、Co2+、Zn2+等掺杂，现在用一价离子进行掺杂。
迄今仅知道，以磁铁铅矿结构结晶的化合物仅能用二价离子或者一价和三价离子的混合物进行掺杂。
现在令人惊奇地发现，在烧结过程中用Li掺杂往往有利地形成断裂裂纹。在专业领域中已知Li2O作为烧结助剂。但是在制备隔热层时强烈的烧结通常被评价为是不利的。强烈的烧结通常导致刚性升高，这进而促进层的剥落。与用MgO掺杂相比，在用Li掺杂时尽管表现出强烈的和长时间烧结，但不会不利地损害刚性。在烧结期间在层中所出现的应力裂纹通常导致相对于相邻设置的构件的应力容差升高。
特别有利的隔热材料构造尤其为以镧作为M1元素和以铝作为M2元素的化合物。在这种用Li掺杂的六铝酸镧情况下发现了特别有利的LaLiAl11O18.5形式的组合物。但是，此外，组合物LaLi0.5Al11.5O19也非常适合用作隔热层。
通过施加本发明的隔热材料，可以在高热负载的构件上施加薄和非常高效的隔热层，所述隔热层是特别长时间稳定的和在交替温度负载情况下通常阻止层的剥落。
所述材料原则上也适合用于制造整块构件或者用作陶瓷泡沫。
作为施加方法特别合适的是热喷镀方法和PVD/CVD方法。
其中梯度层构造原则上也是可行的和适用的。
具体描述部分
下面参照示例性实施方案和两幅附图详细阐述本发明，但并不由它们限制本发明的主题。
对于LaLiAl11O18.5的等离子体喷镀实验，使用了喷雾干燥的空心球粉末。其既可以作为在其下具有粘合涂层的单层使用，又作为和YSZ的混合物使用。
最重要的是其中示出下面复合材料：
1.粘合涂层(100-150μm)，朝向金属叶片的最低层
2.YSZ(150-200μm)
3.LaLiAl11O18.5(150μm)，最上层
以这种方式通过等离子体喷镀施加的单层参见图1中的LaLiAl11O18.5的显微照片。
LaLiAl11O18.5的制备可以通过湿化学沉淀物淀积或者作为氧化物的固体反应进行。对于固体反应而言，称量化学计量量的La2O3、α-Al2O3和Li2O或者Li2CO3(其是廉价的)，在乙醇中混合，并研细直至d50＝1.5μm的粒径。这种混合物经干燥，然后在至少1450℃的温度下反应。NdLiAl11O18.5和GdLiAl11O18.5的制备类似于上述描述进行，区别在于使用Nd2O3或者Gd2O3。所述NdLiAl11O18.5具有弱的淡紫色-蓝色，而LaLiAl11O18.5和GdLiAl11O18.5作为白色粉末存在。
由此获得的化合物基本以具有如下晶格常数的六方晶系磁铁铅矿结构结晶：
La的情况，a，b＝556.33±0.55pm，c＝2193.07±2.86pm，
Nd的情况，a，b＝541.21±0.85pm，c＝2190.01±3.46pm，
Gd的情况，a，b＝514.51±0.76pm，c＝2193.07±3.24pm，
α，β＝90°，γ＝120°。
图2示出了LaLiAl11O18.5的X射线衍射图。灰色箭头指出了少量的LaAlO3杂质。
在制备LaLiAl11O18.5时常常获得多相(类似于在LaMgAl11O19的情况)。除了磁铁铅矿结构之外，可以出现的典型化合物是α-Al2O3、LaAlO3和LiAl5O8(假尖晶石)。本发明的粉末产物含有极低量的这些组分中的一种或两种。在大多数情况下，出现副相是没有最优化的均一性和/或炉温过低的证据。
副相本身在极低量情况下仍不产生干扰。但是，特别地，大于10％的较大量LaAlO3通常会降低隔热层的寿命和因此应当避免。少量的杂质α-Al2O3是无关紧要的。
高于1000℃时，LaLiAl11O18.5的导热率为3.78Wm-1K-1，与YSZ(2.3Wm-1K-1)相比明显更高。尽管如此，这种材料仍适合用作隔热层。这里所述值是对于块状材料测定的。在等离子体喷镀层情况下，通常还会出现导热率的显著下降。
LaLiAl11O18.5的热膨胀系数为8.5-10.5*10-6，比YSZ更小。这对于用作隔热材料是不利的。然而，在此占主要地位的是形成断裂裂纹的明确优点，其导致热膨胀的重要性丧失。
图3和4示出了在图1中示出的同一样品在不同放大倍数下的SEM(扫描电子显微镜)照片。断裂边缘的微观结构明显不同于示例性的等离子喷镀锆涂层。
图5示出了于1200℃热处理(真空)5小时后在LaLiAl11O18.5等离子体喷镀层中形成的典型断裂裂纹。

Claims (12)

1.隔热材料，包括第一相，该第一相接化学计量含有0.1-10mol％M12O3、0.1-10mol％Li2O以及作为其余物的M22O3和附带杂质，其中M1选自元素镧、钕、钆或者它们的混合物，M2选自元素铝、镓、铁或它们的混合物，其中第一相以磁铁铅矿结构存在。
2.权利要求1的隔热材料，其具有至少一个组成为M1M2O3、LiM22O3、LiM25O8或者Li2O的其它相。
3.权利要求1或2的隔热材料，具有第一相，所述第一相按化学计量含有1-10mol％M12O3、0.5-10mol％Li2O以及作为其余物的M22O3和附带杂质。
4.权利要求1-3的隔热材料，具有第一相，所述第一相按化学计量含有3-8mol％M12O3、0.5-8mol％Li2O以及作为其余物的M22O3和附带杂质。
5.权利要求1-4的隔热材料，其中第一相含有La2O3作为M12O3。
6.权利要求1-5的隔热材料，其中第一相含有3-8mol％La2O3、0.5-7.8mol％Li2O以及作为其余物的Al2O3、Ga2O3或者Fe2O3。
7.权利要求1-6的隔热材料，其中第一相具有LaLiAl11O18.5或者LaLi0.5Al11.5O19的组成。
8.权利要求1-7的隔热材料，其中第一相含量占隔热材料的至少80重量％。
9.权利要求8的隔热材料，其中所述第一相含量占隔热材料的至少90重量％。
10.权利要求1-9的隔热材料在隔热层中的用途。
11.权利要求10的用途，与YSZ一起用于隔热层。
12.用于制备根据权利要求1-9的隔热材料的方法，该方法具有以下步骤：
-在溶剂中混合化学计量量的M12O3、Li2O或者Li2Co3以及M22O3，并研细，
-干燥该混合物并使其在至少1450℃的温度下进行反应，
-然后在固体反应中形成隔热材料。
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