CN116964238A - 用于陶瓷基复合材料的氧化屏障材料和方法 - Google Patents

用于陶瓷基复合材料的氧化屏障材料和方法 Download PDF

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CN116964238A
CN116964238A CN202280013564.1A CN202280013564A CN116964238A CN 116964238 A CN116964238 A CN 116964238A CN 202280013564 A CN202280013564 A CN 202280013564A CN 116964238 A CN116964238 A CN 116964238A
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apparent density
rare earth
environmental barrier
coating
hthv
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陈殿营
A·佩格勒
G·维福迪
M·R·多尔福曼
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Oerlikon Metco US Inc
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Abstract

施加环境屏障涂层的方法和环境屏障涂层。该方法包括经由高温及高速(HTHV)工艺施加高表观密度粉末。高表观密度粉末包含稀土硅酸盐、莫来石或碱性硅酸盐中的至少一种。

Description

用于陶瓷基复合材料的氧化屏障材料和方法
背景
1.发明领域
用以产生密封的环境屏障涂层(EBC)的材料和方法，以避免由热生长的SiO2氧化物(TGO)引起的散裂。
2.背景信息讨论
已将环境屏障涂层(EBC)施加到基于硅的陶瓷基复合材料(CMC)上，用以保护CMC免于氧化和水蒸气攻击。目前，现有技术EBC体系含有Si粘结涂层和稀土二硅酸盐中间层和/或顶涂层。稀土二硅酸盐具有与底下的SiC基材严密匹配的热膨胀系数(CTE)。在高温燃气涡轮发动机环境中，水蒸气可穿透涂层中产生的微裂纹，以加速Si粘结涂层的氧化，这在热生长氧化物(TGO)到达域值厚度时引起EBC的散裂。由于这种由热生长的SiO2氧化物(TGO)引起的环境屏障涂层(EBC)的散裂是关键的EBC失效模式，因此重要的是，控制TGO生长速率，以便于改进涂层耐久性。
常规地，空气等离子喷涂(APS)工艺通常用于沉积稀土硅酸盐涂层。然而在APS工艺中，颗粒速度通常较低(＜200m/s)，这引起显著的SiO2损失，并导致稀土单硅酸盐相包括在沉积的二硅酸盐涂层中。由于单硅酸盐通常具有比二硅酸盐的CTE(＝4.1x10-6/℃)大得多的CTE(＝7.5x10-6/℃)，因此较大CTE单硅酸盐相包括在二硅酸盐涂层中将会在热循环期间产生裂纹。此类裂纹在涂层中的存在将为氧化物类提供到硅粘结涂层的运送路径，并且导致TGO的迅速生长和涂层的较早失效。因此，控制二硅酸盐涂层中的相组成对于实现高度耐久的EBC是关键性的。另外，孔隙率和微裂纹总是存在于常规的APS EBC中，这将促进氧化剂通过这些微裂纹的扩散，并且加速硅粘结涂层氧化，并因此降低EBC耐久性。
概述
为了降低TGO生长速率，需要密封的氧化屏障层来防止氧化剂扩散到硅粘结涂层表面。
实施方案涉及用以产生密封EBC的材料和方法。此类沉积的密封EBC在高温下，在蒸汽环境中显示出优异的耐氧化性，其中在1316℃下暴露在蒸汽环境中410小时之后几乎没有TGO生长。
实施方案涉及使用示例性高表观密度原料作为EBC材料或原材料，其中按照ASTMB212将“高表观密度”定义为高于1.8g/cc。示例性高表观密度粉末可具有实心陶瓷芯，期望其防止涂覆过程中的SiO2损失。此外，高温(其中所有测量颗粒温度或平均测量颗粒温度高于材料组合物的熔融温度)、高速(其中平均测量颗粒速度大于或等于200m/s)涂覆工艺(HTHV)用来沉积示例性EBC。该HTHV工艺中等离子射流中的颗粒速度超过200m/s，且优选介于400m/s和800m/s之间，以产生致密涂层。作为非限制性举例，根据实施方案的示例性高表观密度粉末可以是Yb2Si2O7原料或粉末。
按照实施方案，已发现，对于使用示例性高表观密度粉末形成的HTHV涂层，在1316℃下暴露在蒸汽环境中410小时之后几乎没有TGO生长。
高温、高速(HTHV)热喷涂工艺可用于在基材上沉积示例性涂层，作为非限制性举例，稀土硅酸盐EBC沉积，优选二硅酸盐EBC沉积。例如，由于通过HTHV施加工艺实现的较高颗粒速度(>200m/s)大于可利用常规APS工艺获得的颗粒速度，因此沉积了致密且无微裂纹的EBC。这种致密微结构提供了针对氧化剂(即，蒸汽、氧气)的扩散屏障，并因此防止硅粘结涂层的氧化。此外，实验结果已证明，对于使用高温及高速(HTHV)工艺制备的示例性涂层，在1316℃下暴露在蒸汽环境中410小时之后几乎没有TGO生长。作为非限制性举例，示例性稀土硅酸盐涂层可以是Yb2Si2O7/Si涂层。
为防止等离子射流中含二氧化硅的熔融颗粒(例如稀土硅酸盐、优选二硅酸盐和莫来石)的显著SiO2损失，优选高表观密度粉末原料或使用高表观密度粉末作为原材料制备的原料粉末。该高表观密度粉末具有实心陶瓷芯，期望其防止涂覆过程中的SiO2损失。优选的表观密度超过1.8g/cc，优选超过2.2g/cc。
高表观密度粉末或使用高表观密度粉末制备的粉末具有11μm-125μm，优选11μm-62μm的粒度分布。
使用高表观密度粉末原料，经HTHV沉积的Yb2Si2O7涂层中存在例如仅仅～6.0v％的Yb2SiO5相，这有利于保持涂层的CTE与基材的CTE相匹配。
可使用以下工艺来制造高表观密度粉末：
1.熔融/破碎；
2.附聚并烧结；和/或
3.附聚并等离子致密化。
高温及高速热喷涂工艺可以是以下工艺中的任意种，并且可在空气气氛中操作或在真空气氛中操作。
1.高温、高速大气等离子喷涂工艺；
2.高温、高速真空等离子喷涂工艺；或
3.高温、高速氧燃料喷涂工艺。
在任何以上工艺中，飞行颗粒的平均速度超过200m/s，优选超过400m/s。此外，在高温、高速真空等离子喷涂工艺中，真空范围为1mbar-100mbar。
根据实施方案的高表观密度粉末原料可具有以下化学组成：
1.稀土硅酸盐，优选二硅酸盐，例如RE2Si2O7，其中RE可以是Y、La、Ce、Sc、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的任意种；
2.莫来石；
3.碱性硅酸盐(BaO-SrO-Al2O3-SiO2)；
4.具有另外的0.5wt％-10wt％的SiO2混合物的以上化学组成(1-3)中的任意种。
5.热膨胀系数范围为3.5x10-6/k-6x10-6/k的材料。
6.以上者的任意组合。
本发明的其它示例性实施方案和优点可通过审阅本公开内容和附图来确定。
附图简述
在下面的详述中，参考作为本发明的示例性实施方案的非限制性举例所提及的多幅附图，进一步描述了本发明，其中遍及附图的若干视图中，相似的附图标记代表相似的部件，并且其中：
图1A示出了使用熔融/破碎方法制备的示例性粉末；
图1B示出了使用附聚并烧结的方法制备的示例性粉末；
图2A示出了使用图1A的示例性粉末的预合金化的熔融/破碎的粉末制备的附聚并烧结的粉末；
图2B示出了使用图1B的示例性粉末的预合金化的附聚并烧结的粉末制备的附聚并烧结的粉末；
图3A和3B是对常规APS工艺所得到的TGO与根据本发明的高温、高速工艺所得到的TGO进行比较的SEM图像；
图4是对使用常规APS工艺所形成的示例性涂层中的相组成与使用根据本发明的高温、高速工艺所形成的示例性涂层的相组成进行比较的表；以及
图5示出了根据本发明的涂层实例。
详述
本文所显示的细节作为举例并且仅用于例示性讨论本发明实施方案的目的，并且是为了提供据信是本发明的原理和概念方面的最有用和最容易理解的描述而呈现的。在这方面，不试图比基本理解本发明所必需的更详细地来显示本发明的结构细节，结合附图的描述使得如何可以在实践中体现本发明的若干形式对于本领域技术人员而言是显而易见的。
为防止等离子射流中含二氧化硅的熔融颗粒(例如稀土硅酸盐，优选二硅酸盐和莫来石)的显著SiO2损失，优选高表观密度粉末原料或使用高表观密度粉末作为原材料所制备的原料粉末。高表观密度粉末具有实心陶瓷芯，期望其防止涂覆过程中的SiO2损失。优选的表观密度超过1.8g/cc，优选超过2.2g/cc。
可使用以下工艺来制造高表观密度粉末：
1.熔融/破碎；
2.附聚并烧结；和/或
3.附聚并等离子致密化。
此外，根据这些工艺制备的粉末的相纯度超过95v％。
图1A和图1B示出了高表观密度且高相纯度的粉末。如图1A中所显示，可使用熔融/破碎方法来制备示例性高表观密度粉末，例如稀土硅酸盐，例如Yb2Si2O7粉末。此类熔融/破碎的示例性Yb2Si2O7粉末的表观密度大于2.2g/cc。图1B示出了可使用附聚并烧结的方法来制备的高表观密度粉末，例如稀土硅酸盐，例如Yb2Si2O7粉末。此类附聚并烧结的示例性Yb2Si2O7粉末的表观密度超过2.4g/cc。图1A和图1B的粉末的相纯度超过95v％。
图2A和图2B示出了使用以上高表观密度且高纯度的粉末(即，预合金化粉末)作为原材料制备的示例性粉末。因此，除了直接使用上文描述的高表观密度且高相纯度的粉末作为用于热喷涂EBC的原料之外，还可使用这些高表观密度且高相纯度的预合金化粉末作为用于相对较低表观密度粉末制造的原材料。在这些实施方案中，将图1A和图1B中示出的高表观密度且高相纯度的粉末碾磨至尺寸小于10μm，优选小于3μm，且然后可使这些更细微的粉末附聚并烧结至所需的范围为11μm-105μm、优选11μm-62μm的粒度分布。图2A示出了使用图1A的预合金化的熔融/破碎的粉末制备的附聚并烧结的示例性粉末，例如稀土硅酸盐，例如Yb2Si2O7粉末。该附聚并烧结的示例性Yb2Si2O7粉末的表观密度超过1.4g/cc。图2B示出了使用图1B的预合金化的附聚并烧结的粉末制备的附聚并烧结的示例性粉末，例如稀土硅酸盐，例如Yb2Si2O7涂层。此类附聚并烧结的示例性Yb2Si2O7粉末的表观密度超过1.6g/cc。这些实施方案中的优点在于使用预合金化的较高表观(密度)粉末作为原材料制备的这些低表观密度粉末可防止在高温喷涂过程中从颗粒中损失SiO2，并且可产生高纯度涂层，以致利用HTHV工艺，可使用这些低表观(密度)粉末制备致密涂层。
此外，示例性高表观密度粉末或预合金化处理的示例性高表观密度粉末原料不限于上文确认的稀土硅酸盐，但是可具有以下化学组成：
1.稀土硅酸盐，优选二硅酸盐，例如RE2Si2O7，其中RE可以是Y、La、Ce、Sc、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu中的任意种；
2.莫来石；
3.碱性硅酸盐(BaO-SrO-Al2O3-SiO2)；
4.具有另外的0.5wt％-10wt％的SiO2混合物的以上化学组成(1-3)中的任意种。
5.热膨胀系数范围为3.5x10-6/k-6x10-6/k的材料。
6.以上者的任意组合。
可使用高温、高速(HTHV)热喷涂工艺来沉积根据实施方案的高表观密度粉末，以形成EBC。由于该HTHV工艺产生的颗粒速度(＞200m/s)高于可通过常规APS工艺实现的颗粒速度，因此已发现，沉积了致密(例如＜5％孔隙率)且无微裂纹的EBC。该致密微结构为氧化剂(即，蒸汽、氧气)提供了扩散屏障，并因此防止硅粘结涂层的氧化。优选地，HTHV工艺产生大于400m/s的颗粒速度。
此外，HTHV热喷涂工艺可以是以下工艺中的任意种，并且可以在空气气氛中操作或在真空气氛中操作。
1.高温、高速大气等离子喷涂工艺；
2.高温、高速真空等离子喷涂工艺；或
3.高温、高速氧燃料喷涂工艺。
在任何以上工艺中，飞行颗粒的平均速度超过200m/s，优选超过400m/s。此外，在高温、高速真空等离子喷涂工艺中，真空范围为1mbar-100mbar。
图3A和图3B示出了用以比较在1316℃下将示例性EBC体系(例如Yb2Si2O7/Si EBC体系)暴露于90％H2O-10％O2环境中410小时之后的TGO生长的SEM图像。图3A的SEM图像(其显示使用常规低速APS工艺制备的Yb2Si2O7/Si EBC体系)显示出在Si粘结涂层与施加的Yb2Si2O7层之间的～11μm厚的TGO。对照之下，图3B的SEM图像(其显示使用高温高速(HTHV)工艺制备的Yb2Si2O7/Si EBC体系)在Si粘结涂层与Yb2Si2O7层之间几乎显示不出可辨别的TGO生长。
图4提供了对用常规低速工艺制备的示例性涂层的相组成与用高速HTHV工艺制备的示例性涂层的相组成进行比较的表，该示例性涂层例如为稀土硅酸盐涂层，例如Yb2Si2O7。从该表中显示了，低速APS沉积的Yb2Si2O7(二硅酸盐)涂层的相组成包括～38.0v％的Yb2SiO5(单硅酸盐)相，而仅～6.0v％的Yb2SiO5(单硅酸盐)相存在于HTHV沉积的Yb2Si2O7(二硅酸盐)涂层中。因为该单硅酸盐Yb2SiO5的CTE(＝7.5x10-6/℃)比二硅酸盐Yb2Si2O7的CTE(＝4.1x10-6/℃)大得多，所以相比于通过APS工艺沉积的涂层，通过HTHV工艺沉积的二硅酸盐涂层中CTE单硅酸盐相的体积减小将产生致密且无微裂纹的EBC，前者工艺在热循环期间生成裂纹，以产生氧化物类到硅粘结涂层的运送路径。因此，控制按照所公开的实施方案的二硅酸盐涂层中的相组成是有利的，以便于实现高度耐久的EBC。然而，应理解，可经由上文讨论的高速HTHV工艺有利地利用一些具有低CTE的稀土单硅酸盐作为EBC。
按照实施方案，图5示出了按照实施方案的涂层实例。示例性涂层形成在例如SiC或Si3N4的基材上，基材的厚度大于40mil。示例性涂层可包括沉积在基材上的粘结涂层，其厚度为2μm-500μm，且优选25μm-200μm。可通过热喷涂工艺(例如APS、HTHV或真空等离子喷涂)或通过物理气相沉积工艺或通过化学气相沉积工艺来施加该粘结涂层，以具有小于10％且优选小于5％的孔隙率。此外，粘结涂层可具有以下化学组成：
1.Si；
2.Si-氧化物，例如Al2O3、B2O3、HfO2、TiO2、TaO2、BaO、SrO；
3.硅化物，例如RESi、HfSi2、TaSi2、Ti2Si2；
4.RE2Si2O7-Si；
5.RE2Si2O7-硅化物；
6.莫来石-Si
7.莫来石-硅化物
8.以上者的组合。
此外，RE可以是Y、La、Ce、Sc、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu中的任意种。
示例性涂层还可包括形成在粘结涂层上以阻挡氧气和蒸汽扩散的氧化屏障层。沉积在粘结涂层上的氧化屏障层的厚度可以为10μm-1000μm，且优选50μm-250μm。根据实施方案，通过HTHV工艺施加该氧化屏障层，以具有小于10％且优选小于5％的孔隙率。此外，氧化屏障层可具有以下化学组成：
1.稀土硅酸盐，优选二硅酸盐，例如RE2Si2O7，其中RE可以是Y、La、Ce、Sc、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu中的任意种；
2.莫来石
3.碱性硅酸盐(BaO、SrO、Al2O3或SiO2)；
4.具有另外的0.5wt％-10wt％的SiO2混合物的1-3的化学组成；
5.热膨胀系数范围为3.5x10-6/k-6x10-6/k的材料；
6.以上者的任意组合。
注意到，前述实例仅出于解释的目的而提供，并且决不解释为限制本发明。虽然已经参考示例性实施方案描述了本发明，但是应理解，本文中使用的词语是描述和例示性词语，而非限制性词语。在不背离本发明各方面的范围和精神的情况下，在所附权利要求书的范围内，可以做出如目前所陈述和修改的改变。虽然本文已经参考特定的手段、材料和实施方案描述了本发明，但是本发明不意欲限于本文中公开的细节；相反，本发明扩展到所有功能上等同的结构、方法和用途，例如在所附权利要求书的范围内。
权利要求书(按照条约第19条的修改)
1.一种施加环境屏障涂层的方法，其包括：
经由高温及高速(HTHV)工艺施加高表观密度粉末，
其中所述高表观密度粉末的表观密度大于1.8g/cc，其包含稀土硅酸盐、莫来石或碱性硅酸盐中的至少一种，并且
其中所述高表观密度粉末的粉末具有实心陶瓷芯。
2.根据权利要求1所述的方法，其中所述碱性硅酸盐包含BaO、SrO、Al2O3或SiO2。
3.根据权利要求1所述的方法，其中所述高表观密度粉末进一步包含0.5wt％-10wt％的SiO2混合物。
4.根据权利要求1所述的方法，其中所述高表观密度粉末进一步包含热膨胀系数范围为3.5x10-6/k-6x10-6/k的材料。
5.根据权利要求1所述的方法，其中所述HTHV工艺产生大于200m/s的颗粒速度。
6.根据权利要求5所述的方法，其中所述HTHV工艺产生大于400m/s的颗粒速度。
7.根据权利要求1所述的方法，其中所述HTHV工艺包括以下工艺之一：高温、高速大气等离子喷涂工艺；高温、高速真空等离子喷涂工艺；或高温、高速氧燃料喷涂工艺。
8.根据权利要求1所述的方法，其中所述稀土硅酸盐包含二硅酸盐。
9.根据权利要求8所述的方法，其中所述二硅酸盐包含RE2Si2O7，其中RE可以是Y、La、Ce、Sc、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu中的任意种。
10.根据权利要求1所述的方法，其中所述稀土硅酸盐包含低热膨胀系数单硅酸盐。
11.一种环境屏障涂层，其包含：
包含稀土硅酸盐、莫来石或碱性硅酸盐中的至少一种的致密涂层。
12.根据权利要求11所述的环境屏障涂层，其中所述碱性硅酸盐包含BaO、SrO、Al2O3或SiO2。
13.根据权利要求11所述的环境屏障涂层，其中所述高表观密度粉末进一步包含0.5wt％-10wt％的SiO2混合物。
14.根据权利要求11所述的环境屏障涂层，其中所述高表观密度粉末进一步包含热膨胀系数范围为3.5x10-6/k-6x10-6/k的材料。
15.根据权利要求11所述的环境屏障涂层，其中所述稀土硅酸盐包含二硅酸盐。
16.根据权利要求15所述的环境屏障涂层，其中所述二硅酸盐包含RE2Si2O7，其中RE可以是Y、La、Ce、Sc、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu中的任意种。
17.根据权利要求11所述的环境屏障涂层，其中所述稀土硅酸盐包含低热膨胀系数单硅酸盐。
18.根据权利要求1所述的方法，其中所述表观密度大于2.2g/cc。
19.根据权利要求1所述的方法，其中所述高表观密度粉末的粉末的粒度分布介于15μm和125μm之间。
20.根据权利要求19所述的方法，其中所述高表观密度粉末的粉末的粒度分布介于15μm和62μm之间。

Claims (17)

1.一种施加环境屏障涂层的方法，其包括：
经由高温及高速(HTHV)工艺施加高表观密度粉末，
其中所述高表观密度粉末包含稀土硅酸盐、莫来石或碱性硅酸盐中的至少一种。
2.根据权利要求1所述的方法，其中所述碱性硅酸盐包含BaO、SrO、Al2O3或SiO2。
3.根据权利要求1所述的方法，其中所述高表观密度粉末进一步包含0.5wt％-10wt％的SiO2混合物。
4.根据权利要求1所述的方法，其中所述高表观密度粉末进一步包含热膨胀系数范围为3.5x10-6/k-6x10-6/k的材料。
5.根据权利要求1所述的方法，其中所述HTHV工艺产生大于200m/s的颗粒速度。
6.根据权利要求5所述的方法，其中所述HTHV工艺产生大于400m/s的颗粒速度。
7.根据权利要求1所述的方法，其中所述HTHV工艺包括以下工艺之一：高温、高速大气等离子喷涂工艺；高温、高速真空等离子喷涂工艺；或高温、高速氧燃料喷涂工艺。
8.根据权利要求1所述的方法，其中所述稀土硅酸盐包含二硅酸盐。
9.根据权利要求8所述的方法，其中所述二硅酸盐包含RE2Si2O7，其中RE可以是Y、La、Ce、Sc、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu中的任意种。
10.根据权利要求1所述的方法，其中所述稀土硅酸盐包含低热膨胀系数单硅酸盐。
11.一种环境屏障涂层，其包含：
包含稀土硅酸盐、莫来石或碱性硅酸盐中的至少一种的致密涂层。
12.根据权利要求11所述的环境屏障涂层，其中所述碱性硅酸盐包含BaO、SrO、Al2O3或SiO2。
13.根据权利要求11所述的环境屏障涂层，其中所述高表观密度粉末进一步包含0.5wt％-10wt％的SiO2混合物。
14.根据权利要求11所述的环境屏障涂层，其中所述高表观密度粉末进一步包含热膨胀系数范围为3.5x10-6/k-6x10-6/k的材料。
15.根据权利要求11所述的环境屏障涂层，其中所述稀土硅酸盐包含二硅酸盐。
16.根据权利要求15所述的环境屏障涂层，其中所述二硅酸盐包含RE2Si2O7，其中RE可以是Y、La、Ce、Sc、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb或Lu中的任意种。
17.根据权利要求11所述的环境屏障涂层，其中所述稀土硅酸盐包含低热膨胀系数单硅酸盐。
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