CN109251025B - 特别用于燃气涡轮的高温绝热材料及其制造方法 - Google Patents

特别用于燃气涡轮的高温绝热材料及其制造方法 Download PDF

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CN109251025B
CN109251025B CN201810770288.9A CN201810770288A CN109251025B CN 109251025 B CN109251025 B CN 109251025B CN 201810770288 A CN201810770288 A CN 201810770288A CN 109251025 B CN109251025 B CN 109251025B
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hafnium oxide
particles
clusters
diameter
yttria
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CN109251025A (zh
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H-P.博斯曼
D.雷努施
T-T.楚
M.米彻勒
J.库尔伯勒
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Ansaldo Energia IP UK Ltd
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Abstract

提供一种高温绝热材料，特别是用于燃气涡轮部件的高温绝热材料，包括：具有多孔微观结构的氧化钇稳定化氧化锆(YSZ)的多孔陶瓷基体；和以聚集簇的形式掺入所述多孔陶瓷基体内的二氧化铪(HfO2)颗粒。

Description

特别用于燃气涡轮的高温绝热材料及其制造方法
优先权主张
本申请主张在2017年7月14日提交的欧洲专利申请号17181554.1的优先权，其公开内容通过引用并入。
技术领域
本发明涉及一种高温绝热材料、特别是用于燃气涡轮部件的高温绝热材料，及其制造方法。
特别地，本发明涉及一种适合于替代目前的热障涂层(TBC)的材料。
背景技术
在许多技术领域中，例如在燃气涡轮领域中，众所周知需要对在非常高的温度下操作的部件/表面进行有效的热防护。
特别地，在燃气涡轮中，内部部件暴露于特别有侵蚀性的环境，使得部件承受高水平的应力，不仅有热应力，而且有腐蚀和机械应力。
根据通常的方法，燃气涡轮部件由具有被热障涂层(TBC)保护的表面的专门设计的金属合金(例如所谓的超合金)制成。
这种涂层借助于绝热材料隔离部件，所述绝热材料可以经受住载荷金属表面与涂层表面之间的显著温差。
例如，已知由部分稳定化的氧化锆陶瓷制成的热障涂层。
然而，对于这种涂层，在高温应用的范围方面也存在限制；此外，经涂布部件的制造相当复杂和昂贵；且涂层不可避免地增加部件的寄生重量，这特别对于旋转/移动部件是不合乎需要的。
因此，由于对更高温度操作(在更高温度下效率增加)、更好的耐用性/寿命、较不昂贵和更有效的部件的需求增加，用不同种类的热防护系统替代TBC存在很大的动力。
另一种已知的方法是基于陶瓷材料的使用，例如以盖面瓷砖的形式。
然而，即使已知陶瓷材料通常具有低导热率，目前可用的材料仍具有改进的空间，特别是为了提高操作温度，降低导热率，延长预期寿命，增加对机械和化学应力的抵抗力。
发明内容
因此，本发明的一个目的是提供一种适合于克服现有技术中的上述问题的高温绝热材料及其制造方法。
特别地，本发明的一个目的是提供一种与传统陶瓷相比具有改进的性质和性能的材料，以便适合于替代传统的TBC，特别是在燃气涡轮部件中。
因此，本发明涉及如权利要求1中限定的高温绝热材料，以及如权利要求12中限定的制造高绝热材料的方法。
本发明的有利的优选特征是从属权利要求的主题。
基本上，本发明提供一种特别适合于燃气涡轮部件的热防护的、改进的高温绝热材料，包括具有多孔微观结构的基础YSZ陶瓷基体和分散在其中的二氧化铪颗粒；二氧化铪颗粒以聚集簇的形式掺入在多孔陶瓷基体内。
(众所周知：氧化锆(zirconia)是氧化锆(zirconium oxide)，ZrO2；氧化钇(yttria)是三氧化二钇(yttrium oxide)，Y2O3；二氧化铪(hafnia)是氧化铪(IV) (hafnium(IV) oxide)，即二氧化铪，HfO2)。
基础陶瓷基体由氧化钇稳定化氧化锆、特别是完全稳定化的YSZ组成。
有利地，氧化钇稳定化氧化锆是完全稳定化的氧化钇稳定化氧化锆，其氧化钇含量为8-14重量%范围。
根据本发明，掺入二氧化铪颗粒不是为了改进陶瓷材料的机械性质，而是为了增加经受住较高操作温度和降低最终产品的导热率的能力。
因此，有利地将二氧化铪以簇的形式加入到陶瓷基体中，即细二氧化铪颗粒聚集/团聚在一起以形成更大的簇。二氧化铪簇随机分布在陶瓷基体中。
团聚的二氧化铪簇优选具有约1至30μm，优选约5至20μm，更优选5至10μm的直径，导致复合材料的机械抵抗力降低，但另一方面，随机分布的簇增加在几个热循环中经受住高达约1600℃温度的能力，而没有临界或破坏性裂纹扩展。在烧结过程期间在二氧化铪细粒周围形成的微裂纹被认为是在加热和冷却期间发生的热应力消散的主要原因。
有利地，本发明的材料含有约0.1至10体积%，优选0.5至5.0体积%(相对于YSZ陶瓷基体的体积) 的量的二氧化铪簇。
加入成孔剂产生具有10至40体积%(优选20体积%)的直径为1至10μm的细孔的多孔微观结构。
成孔剂，其优选具有球形颗粒以产生球形孔，例如是球形形式的聚(甲基丙烯酸甲酯)，PMMA。
加入成孔剂主要是为了增加材料的隔离(isolation)特征。
然而，聚集的二氧化铪簇的分散和多孔结构(通过加入成孔剂赋予)二者协同地有助于本发明的材料的特征，且彼此相互作用以提供经受住较高操作温度的改进能力，甚至在侵蚀性(例如氧化)气氛中并进行快速热循环的情况下亦然。
在一些实施方案中，YSZ陶瓷基体还含有至少一种耐高温无机粉末的非聚集细粉末颗粒、特别是二氧化铪细颗粒的分散体。
特别地，细二氧化铪颗粒以1至10体积%(优选2至6体积%) 的量加入，且具有0.1至10μm(优选0.3至1.0μm)的直径，以提供增韧作用和高热稳定性(高达1600℃)。
掺入细尺寸的二氧化铪颗粒(优选具有小于掺入陶瓷基体中的二氧化铪簇的尺度、特别是直径)具有与例如氧化锆增韧的氧化铝(ZTA)中的氧化锆的作用类似的作用。事实上，二氧化铪相对于氧化锆具有类似行为，尽管转变的温度移位到更高的区域。
细二氧化铪颗粒的分散可以部分或完全地由一种或多种其它耐高温无机粉末(如Al2O3或V2O5)的分散替代。
因此，本发明提供一种材料，其与用于燃气涡轮操作条件的已经知道的陶瓷相比时，具有更高的操作温度能力和增强的耐热循环性。
基本上，通过将微孔和具有良好热稳定性的细无机粉末包含在高温陶瓷基体中，已知陶瓷材料的通常低的导热率和高强度得到改进。相对于已知的陶瓷材料，根据本发明的改变导致材料具有较低的导热率和经受住较高操作温度的改进能力，甚至在侵蚀性(例如氧化)气氛中并进行快速热循环的情况下亦然。
因此，本发明的材料完全适用于其中需要耐热应力性和机械强度二者的条件，例如在燃气涡轮中，且可以有效地替代传统的TBC。
本发明的材料可例如用于实现更高的烧制温度和改进的涡轮效率。
例如，本发明的材料可用于制备比已知类型的陶瓷砖具有改进性能的砖，例如由陶瓷基体复合材料(CMC，由嵌入陶瓷基体中的陶瓷纤维组成)制成的砖。
本发明的材料有利地通过包括以下步骤的方法制备：
a)制备均匀粉末混合物，其包含：
- 氧化钇稳定化氧化锆(YSZ)粉末；
- 包含聚集的二氧化铪颗粒的簇的二氧化铪(HfO2)粉末；
- 至少一种成孔剂；
- 至少一种溶剂；
b)热处理所述混合物以产生氧化钇稳定化氧化锆的多孔陶瓷基体，所述多孔陶瓷基体具有多孔微观结构且含有嵌入并分散在多孔陶瓷基体内的二氧化铪簇。
特别地，所述均匀粉末混合物通过研磨制备。
优选地，氧化钇稳定化氧化锆是完全氧化钇稳定化氧化锆，其氧化钇含量为8-14重量%范围。
有利地，由聚集的二氧化铪颗粒制成并随机分布在陶瓷基体中的二氧化铪簇以0.1至10.0体积%，优选0.5至5体积%范围的量加入；且具有约1至30μm，优选约5至20μm，更优选约5至10μm的直径。
有利地，成孔剂以具有约1至10μm范围的平均直径的球形微珠的形式成形。
成孔剂优选以10至40体积%范围的量加入。
成孔剂例如是PMMA。
在一些实施方案中，粉末混合物还含有至少一种耐高温无机粉末的非聚集细粉末颗粒，特别是二氧化铪细颗粒，或Al2O3或V2O5细颗粒。
特别地，细二氧化铪颗粒以1至10体积%(优选2至6体积%)的量加入，且具有0.1至10µm (优选0.3至1.0µm) 的直径。
在研磨步骤之后，本发明的方法进一步包括：
- 干燥步骤，特别是真空干燥步骤，
- 压制步骤，特别是单轴模压步骤，
- 烧尽步骤，
- 烧结步骤。
附图说明
通过以下非限制性实施方案中的实施例，参考附图进一步描述本发明，其中：
- 图1是显示根据本发明的材料的微观结构的显微照片；
- 图2是图1的材料的细节的较高放大倍数的显微照片，特别显示在二氧化铪细粒周围具有裂纹(圆圈区域)的一些二氧化铪簇；
- 图3是显示与具有相同孔隙率含量(20体积%)但没有二氧化铪的相同的基础YSZ相比，在根据本发明且在YSZ基体中分别含有2和5体积%的二氧化铪且具有20体积%的孔隙率的复合材料中的热膨胀的图；
- 图4显示分别含有2和5体积%的粗二氧化铪颗粒的本发明的材料(方形)和含有2体积%的细粒二氧化铪颗粒的材料(点)的样品的挠曲强度(通过四点弯曲强度方法测量)。
具体实施方式
如前所述，根据本发明的材料是包含完全稳定化氧化锆(特别是完全氧化钇稳定化氧化锆(YSZ))的陶瓷基体的复合材料，其中分散有团聚的二氧化铪颗粒，且具有通过加入至少一种成孔剂获得的细孔(具有预定尺寸)的多孔结构。
有利地，二氧化铪颗粒是团聚颗粒，即聚集在一起呈颗粒的簇的颗粒。簇均匀地分散在陶瓷基体中。
任选地，该材料还包括细尺寸的二氧化铪颗粒(或另一种类似的耐高温无机粉末)。
本发明的陶瓷复合材料可以例如通过通常用于制造陶瓷材料的一般类型的制造方法制备，特别是干法，包括无压烧结步骤，然后是单轴模压步骤。
更详细地，根据本发明的材料的示例性实施方案如下制备。
首先制备粉末混合物，其包含：
- 氧化钇稳定化氧化锆(YSZ)；
- 二氧化铪(HfO2)；
- 成孔剂，特别是PMMA；
- 溶剂(例如异丙醇)。
特别地，YSZ是完全氧化钇稳定化氧化锆，其氧化钇含量为8至14重量%范围(即氧化钇的重量分数为全部混合物的8至14%)；且密度范围为4至8gcm-3，优选为5至7gcm-3。
例如，本发明的材料含有由Tosoh Europe B.V.提供并标识为“TZ-8YS”的商品YSZ，它是一种完全稳定化的、易模塑级氧化锆，具有5.9gcm-3的密度且含有8mol%氧化钇。
将二氧化铪以聚集颗粒的簇的形式加入到粉末混合物中。
优选地，加入到粉末混合物中的二氧化铪基本上是纯的；特别地，二氧化铪具有高于98%，更优选高于99%且特别是高于99.90%的纯度。
例如，使用具有99.95%的纯度的二氧化铪，其典型密度为约9.68gcm-3。
相对于氧化锆的体积，将二氧化铪簇以优选0.1至10.0体积%，更优选0.5至5体积%范围的量加入到YSZ陶瓷基体中。
固体PMMA，例如具有约1.2gcm-3的密度的PMMA，用作颗粒形式的成孔剂；特别地，PMMA以微珠的形式成形，优选为球形。例如，PMMA由基本上球形的颗粒组成，其平均直径为约1至10μm范围，且优选约6μm。例如，使用具有约6μm粒径的PMMA6。
然而，另一种成孔剂可以替代PMMA，例如另一种合适的等价聚合物。
成孔剂，例如PMMA，以优选10至30体积%范围，更优选15至25体积%，例如约20体积%的量加入。
然后研磨粉末混合物，例如在PVC罐中且使用氧化锆球(例如具有约3mm的直径) 。
陶瓷(YSZ基体与二氧化铪簇的分散体)与成孔剂颗粒(例如PMMA)的均匀粉末混合物是适合于陶瓷材料的粉末或浆料生产的中间产品。
例如，混合物经受：
- 真空干燥步骤，
- 单轴模压步骤，
- 烧尽步骤，
- 烧结步骤。
例如，烧尽步骤通过将材料加热(以约1℃/min的速率提高温度)至950℃，并通过将该温度保持5小时来进行。
在冷却步骤(至室温)之后，对材料进行烧结步骤，例如通过将材料加热(以约4℃/min的速率提高温度)至1600℃且通过保持1600℃的温度1小时来进行；然后，将材料以1.5℃/min的速率冷却至1000℃；且然后以10℃/min的速率冷却至室温。
在YSZ陶瓷基体(特别是14YSZ)中包含5体积% HfO2且孔隙率为20体积%(由相应量的PMMA6产生)的复合陶瓷材料的示例性实施方案的微观结构在图1中显示。
图2的较高放大倍数图片特别显示陶瓷基体中的二氧化铪簇，在二氧化铪细粒周围有裂纹(圆圈区域)。
图3显示与具有相同孔隙率含量(20体积%)但没有二氧化铪的YSZ相比，在根据本发明且在YSZ基体中分别含有2体积%和5体积%的二氧化铪的复合材料中的热膨胀。
图4显示与含有2体积%的细粒二氧化铪颗粒并具有相同孔隙率水平的材料(圆点)相比，分别含有2和5体积%的粗二氧化铪颗粒且孔隙率为20体积%的本发明的样品(方形点)的挠曲强度(通过四点弯曲强度方法测量)。
最后，尽管已经关于上述优选实施方案解释本发明，但是应当理解，在不脱离所附权利要求的范围的情况下，可以进行许多其他可能的修改和变化。

Claims (35)

1.高温绝热材料，包括：具有多孔微观结构的氧化钇稳定化氧化锆(YSZ)的多孔陶瓷基体；和以聚集簇的形式掺入所述多孔陶瓷基体中的二氧化铪(HfO2)颗粒，其中二氧化铪簇由聚集的二氧化铪颗粒制成并随机分布在所述陶瓷基体中以及具有1至30μm的直径。
2.根据权利要求1所述的材料，其中二氧化铪簇具有5至20μm的直径。
3.根据权利要求2所述的材料，其中二氧化铪簇具有5至10μm的直径。
4.根据权利要求1-2中任一项所述的材料，其具有0.1至10体积%范围的二氧化铪簇的含量。
5.根据权利要求4所述的材料，其具有0.5至5.0体积%范围的二氧化铪簇的含量。
6.根据权利要求1-2中任一项所述的材料，其具有带有10至40体积%的孔的多孔微观结构。
7.根据权利要求1-2中任一项所述的材料，其中所述氧化钇稳定化氧化锆是完全氧化钇稳定化氧化锆，具有的氧化钇含量为8-14重量%范围。
8.根据权利要求1-2中任一项所述的材料，具有基本上为球形孔的孔，所述孔的直径为1μm至10μm范围。
9.根据权利要求1-2中一项所述的材料，其中所述YSZ陶瓷基体还包含至少一种耐高温无机粉末的非聚集细粉末颗粒的分散体。
10.根据权利要求9所述的材料，其中所述非聚集细粉末颗粒是二氧化铪细颗粒。
11.根据权利要求9所述的材料，其中所述细粉末颗粒具有0.1至10μm范围的直径。
12.根据权利要求11所述的材料，其中所述细粉末颗粒具有0.3至1.0μm范围的直径。
13.根据权利要求9所述的材料，其中所述细粉末颗粒包括HfO2、Al2O3、V2O5中的一种或多种。
14.根据权利要求9所述的材料，含有1至10体积%的量的细粉末颗粒。
15.根据权利要求1所述的材料，所述高温绝热材料用于燃气涡轮部件。
16.制造高温绝热材料的方法，所述方法包括以下步骤：
a)制备均匀粉末混合物，包含：
- 氧化钇稳定化氧化锆(YSZ)粉末；
- 包含聚集的二氧化铪颗粒的簇的二氧化铪(HfO2)粉末；
- 至少一种成孔剂；
- 至少一种溶剂；
b)热处理所述混合物以产生氧化钇稳定化氧化锆的多孔陶瓷基体，所述多孔陶瓷基体具有多孔微观结构且含有嵌入并分散在所述多孔陶瓷基体内的二氧化铪簇，其中二氧化铪簇由聚集的二氧化铪颗粒制成并随机分布在所述陶瓷基体中以及具有1至30μm的直径。
17.根据权利要求16所述的方法，其中所述均匀粉末混合物通过研磨制备。
18.根据权利要求16或17所述的方法，其中二氧化铪簇以0.1至10.0体积%范围的量加入。
19.根据权利要求18所述的方法，其中二氧化铪簇以0.5至5体积%范围的量加入。
20.根据权利要求16或17所述的方法，其中二氧化铪簇具有5至20μm的直径。
21.根据权利要求20所述的方法，其中二氧化铪簇具有5至10μm的直径。
22.根据权利要求16或17所述的方法，其中所述成孔剂是PMMA。
23.根据权利要求16或17所述的方法，其中所述成孔剂以具有1-10μm范围的平均直径的球形微珠的形式成形。
24.根据权利要求16或17所述的方法，其中所述成孔剂以10至40体积%的量加入。
25.根据权利要求16或17所述的方法，其中所述氧化钇稳定化氧化锆是完全氧化钇稳定化氧化锆，具有的氧化钇含量为8-14重量%范围。
26.根据权利要求16或17所述的方法，其中所述粉末混合物还含有至少一种耐高温无机粉末的非聚集细粉末颗粒。
27.根据权利要求26所述的方法，其中所述非聚集细粉末颗粒是二氧化铪细颗粒。
28.根据权利要求26所述的方法，其中所述细粉末颗粒具有0.1至10μm范围的直径。
29.根据权利要求28所述的方法，其中所述细粉末颗粒具有0.3至1.0μm范围的直径。
30.根据权利要求26所述的方法，其中所述细粉末颗粒包括HfO2、Al2O3、V2O5中的一种或多种。
31.根据权利要求26所述的方法，含有1-10体积%的量的细粉末颗粒。
32.根据权利要求17所述的方法，在所述研磨步骤之后包括：
- 干燥步骤；
- 压制步骤；
- 烧尽步骤；
- 烧结步骤。
33.根据权利要求32所述的方法，其中所述干燥步骤是真空干燥步骤。
34.根据权利要求32所述的方法，其中所述压制步骤是单轴模压步骤。
35.根据权利要求16所述的方法，其中所述高温绝热材料用于燃气涡轮部件。
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