CN101302103B - 具有钆-混晶-烧绿石相和氧化物的陶瓷粉末,陶瓷层和层体系 - Google Patents

具有钆-混晶-烧绿石相和氧化物的陶瓷粉末,陶瓷层和层体系 Download PDF

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CN101302103B
CN101302103B CN2008100956556A CN200810095655A CN101302103B CN 101302103 B CN101302103 B CN 101302103B CN 2008100956556 A CN2008100956556 A CN 2008100956556A CN 200810095655 A CN200810095655 A CN 200810095655A CN 101302103 B CN101302103 B CN 101302103B
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R·苏布拉马尼恩
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Abstract

本发明涉及具有钆-混晶-烧绿石相和氧化物的陶瓷粉末，陶瓷层和层体系。绝热的层体系除了良好的绝热性之外也必须要具有很长的绝热层使用寿命。本发明的层体系(1)由具有锆酸钆和铪酸钆组成的混晶的外陶瓷层(13)构成。

Description

具有钆-混晶-烧绿石相和氧化物的陶瓷粉末,陶瓷层和层体系
技术领域
本发明涉及一种具有烧绿石和氧化物的陶瓷粉末、陶瓷层和层体系。
背景技术
这种层体系含有具有基于镍或钴的金属合金的基材。这类产品首先用作燃气涡轮的零件，特别是用作燃气轮机的浆叶或耐热护壳。这些零件会遭受到腐蚀性燃气的热气流腐蚀。因此，它们必须能够保持较高的耐热标准。另外，也需要使这些零件耐氧化和耐腐蚀。尤其对运动的零件，例如燃气涡轮浆叶，但也对静止零件提出进一步的机械要求。在其中使用可耐受热气的零件的燃气涡轮机中，其功率和效率都会随着工作温度升高而增加。为了获得较高的效率和较高的功率，就要在特别是遭受到高温的燃气涡轮机的元件上涂覆一层陶瓷材料。其能起到作为热气流和金属基材之间的绝热层的作用。
涂层防护金属基体不受腐蚀性热气流的腐蚀。并且，现今的零件多数都具有多个分别满足特殊要求的涂层。因此其也就属于一种多层体系。
因为燃气涡轮机的功率和效率随着工作温度增加而增加，因此人们也就总是试图通过改善涂层体系而获得更高的燃气涡轮机效率。
EP0944746B1公开了烧绿石用作绝热层。但是，对于将材料用作绝热层来说，并不只是要求要有良好的绝热性能，而且还要求能良好地结合于基材上。
EP0992603A1中公开了由氧化钆和氧化锆制成的绝热层体系，其应不具有烧绿石结构。
发明内容
因此，本发明的任务在于提供一种具有良好绝热性和良好基材粘结性并因此而具有长使用寿命的陶瓷粉末、陶瓷层和层体系。
该任务可通过如权利要求1、19或20所述的陶瓷粉末、陶瓷层和陶瓷体系来解决。
本发明所基于的认识是，必须要将整个体系视作整体并且不允许相互隔离地来看待和优化各个层，从而获得长的使用寿命。
在从属权利要求中描述了另外一些有益的措施，它们可以以有益的方式任意结合。
本发明的层体系由具有锆酸钆和铪酸钆构成的混晶的外部陶瓷层组成，该混晶具有特别良好的热性能(适合于基材的膨胀系数，较小的导热系数)并且与零件的中间层和基材协调得非常好。
以下引用附图来更详尽地阐述本发明的实施例。
附图说明
图1本发明的层体系，
图2超合金的组成，
图3燃气涡轮机
图4涡轮机浆叶的透视图，和
图5燃烧室的透视图。
具体实施方式
根据陶瓷层13的组成(图1)来例示性地阐述陶瓷粉末的组成。
一般而言，总是可以出现与烧绿石结构A2B2O7化学计量量的偏差。
烧绿石结构具有通式Gdv(ZrxHfy)Oz，其中v≈2，x+y≈2且z≈7。可以通过缺位或少量的有意或无意的掺杂而形成v，x，y和z这种化学计量组成的偏差。
另外，陶瓷粉末还具有锆和/或铪氧化物的二次氧化物(
Figure S2008100956556D00021
)，特别是其含量为0.5wt％至10wt％，更特别为1wt％至10wt％。有意识地将二次氧化物补加到粉末中，也即使其量明显超过二次氧化物的测量技术的可检验极限值，也即是二次氧化物检验极限值的至少两倍值。
二次氧化物的最大含量优选为8wt％，特别是最大为6wt％，并且更特别是在5wt％至7wt％之间。
这一点优选适于氧化锆。
二次氧化物的最大含量同样也优选为3wt％，特别是最大2wt％，且更特别在1.5wt％至2.5wt％之间。
这些含量特别适于氧化铪。
特别优选陶瓷粉末由至少一种烧绿石相和至少一种二次氧化物构成。
根据使用情况的不同，二次氧化物可以只是由氧化铪组成，从而实现更好的绝热性能，或者二次氧化物只由氧化锆构成，以使膨胀系数更好地适于位于其下的层或者适于基材。
氧化铪和氧化锆的有益性能的组合也能通过使用两种二次氧化物来实现。
并且，二次氧化物优选以氧化物的形式存在。
陶瓷粉末可以优选分别任选地含有烧结助剂不超过0.05wt％的氧化硅、不超过0.1wt％的氧化钙、不超过1wt％的氧化钙、不超过0.1wt％的氧化镁、不超过0.1wt％的氧化铁、不超过0.1wt％的氧化铝和不超过0.08wt％的氧化钛。
烧结助剂能促进涂覆之后和/或在更高温度下使用时层的结合。优选所述的陶瓷粉末由烧绿石、二次氧化物和任选地烧结助剂组成。
优选存在两种二次氧化物，特别是氧化铪和氧化锆。
铪酸钆作为粉末具有43wt％至50wt％、优选44.7wt％至47.7wt％的氧化钆和余量的氧化铪和任选地二次氧化物，优选氧化锆，和烧结助剂。锆酸钆作为粉末具有56wt％至63wt％、优选58wt％至61wt％的氧化钆和余量的氧化锆以及任选地二次氧化物，优选氧化铪，和烧结助剂。作为混晶，根据Hf和Ze的比例将这些成分混和。
优选外部的陶瓷层13含有Gdv(HfxZry)Oz，其中v，x+y≈2，z≈7。
也优选外部的陶瓷层13含有Gdv(HfxZry)O7，其中x+y≈2，v≈2。
优选外部的陶瓷层13含有Gd2(HfxZry)Oz，其中x+y≈2，z≈7。
优选陶瓷粉末的烧绿石结构由特别是v≈2、x+y≈2且z≈7的Gdv(HfxZry)Oz组成。
这里，可以采用锆和铪的多种混合比y∶x。
优选采用较大量的锆。
同样也优选采用铪对锆的混合比为10∶90、20∶80、30∶70或40∶60。另外也优选采用铪对锆的混合比为50∶50、60∶40、70∶30、80∶20或90∶10。
对于铪对锆之比的所述内容优选也同样适于x对y之比(Hf∶Zr＝80∶20对应于y∶x＝1.6∶0.4)。
图1所示为本发明的层体系1。
根据陶瓷层13来例示性地阐述陶瓷粉末的组成。
层体系1具有金属基材4，对于高温下的构件该基材特别由基于镍或钴的超合金(图2)组成。
优选直接在基材4上存在MCrAlX型、特别是NiCoCrAlX型的金属结合层7，且其优选具有(11-13)wt％的钴、(20-22)wt％的铬、(10.5-11.5)wt％的铝、(0.3-0.5)wt％的钇(＝X)、(1.5-2.5)wt％的铼和余量的镍，或者优选具有(24-26)wt％的钴、(16-18)wt％的铬、(9.5-11)wt％的铝、(0.3-0.5)wt％的钇(＝X)、(1-1.8)wt％的铼和余量的镍。
特别优选NiCoCrAl结合层7由这两种组合物之一构成。
在该金属结合层7上优选在涂覆其他陶瓷层之前就已经存在一个氧化铝层，或者在操作时形成这样一个氧化铝层(TGO)。在金属结合层7上或者在氧化铝层(未示出)上优选存在内部陶瓷层10，优选是完全或部分稳定化的氧化锆层。优选采用优选含有6wt％-8wt％钇的钇稳定化的氧化锆。同样也可以采用氧化钙、氧化铈或氧化铪以稳定氧化锆。
氧化锆优选作为等离子喷注层涂覆，也可以优选利用电子束蒸发法(EBPVD)涂覆成圆柱形结构。
在TGO上、在结合层7上或内层10上涂覆一个外陶瓷层13，其根据本发明具有由钆、铪和锆构成的具有烧绿石结构的混晶，也即由上述的陶瓷粉末制得。优选陶瓷层13只由陶瓷粉末制得。
优选层13为遭受热气的最外层。
二次氧化物分布于陶瓷层13内，特别优选均匀分布。
层13可以由给出上述组成含量的粉末制得。同样，混晶也可以在涂覆过程中或者通过热处理在涂覆过程之后制得。
内层10的层厚度优选在内层10和外层13的总层厚D的10％至50％之间。
内层10的层厚度更优选在总层厚的10％至40％或者10％至30％之间。
同样也优选使内层10的层厚为总层厚的10％至20％。
同样还优选内层10的层厚度为总层厚的20％至50％或者20％至40％之间。
当内层10在总层厚上的比例为20％至30％之间时，同样也会获得有益的结果。
优选内层10的层厚为总层厚的30％至50％。
同样也优选使内层10的层厚占据总层厚的30％至40％。
同样优选使内层10的层厚为总层厚的40％至50％。
尽管烧绿石相比ZrO2层具有更好的绝热性能，但ZrO2层也可以制为恰好如烧绿石相一般厚。
对于层体系的高温下短时使用，可以将外层13制为比内层10更薄，也即外层13的层厚为由内层10和外层13构成的总层厚度的10％至40％。
内陶瓷层10优选具有的厚度为100μm-200μm，尤其是150μm±10％。
内层10和外层13的总厚度优选为300μm或优选450μm。最大的总层厚优选为800μm或优选最大600μm。
图3例示了燃气涡轮机100的纵剖局部视图。
燃气涡轮机100在内部具有一个围绕旋转轴102旋转放置的带有轴101的转子103，其也称作是涡轮机转动部件。
沿着转子103方向相继设置吸进壳体104，压缩机105，例如环形面的具有多个共轴设置的燃烧器107的燃烧室110、特别优选是环形燃烧室，涡轮机108和排气壳体109。
环形燃烧室110与例如环形的热气通道111相通。在那里，例如有四个相继接通的涡轮级112构成涡轮机108。
每个涡轮级112例如由两个叶片环构成。沿着工作介质113的流动方向看去，跟着在导向叶片栅115的热气通道111内具有由转动叶片120构成的栅125。
导向叶片130在此固定于定子143的内壳138上，与此相反，栅125的转子叶片120则例如借助于涡轮叶轮盘133而设置于转子103上。
连接于转子103上的是发电机或工作机器(未示出)。
在燃气涡轮机100工作时，由压缩机105通过吸进壳体104抽入并压缩空气135。在压缩机105的涡轮机侧那一端上所提供的压缩空气被导入到燃烧器107中并在那里与燃剂混和。然后点燃混合物并在燃烧室110内形成工作介质113。工作介质113从那里沿着热气通道111流动经过导向叶片130和转动叶片120。在转动叶片120上工作介质113膨胀并传递冲量，从而使得转动叶片120驱动转子103并且使转子103驱动连接其上的工作机器。
在燃气涡轮机100工作时，经受热工作介质113的零件要受热。沿着工作介质113流动方向看去的第一涡轮级112的导向叶片130和转动叶片120是除了构成环状燃烧室110内衬的耐热护壳元件之外最为受热的部分。
为了耐受那里的主导温度，可以借助于冷却介质将其冷却。
同样，零件的基材可以具有取向结构，即其是单晶的(SX-结构)或者具有只是纵向取向的晶粒(DS-结构)。
作为零件材料，特别是用于涡轮叶片120、130和燃烧室110构件的材料，采用例如基于铁、镍或钴的超合金。
这些超合金公开于例如EP1204776B1、EP1306454、EP1319729A1、WO99/67435或WO00/44949中；这些文献有关合金化学组成的内容是本发明公开的一部分。
导向叶片130具有一个朝向涡轮机108内壳138的导向叶片根(这里未示出)和一个位于导向叶片根对面的导向叶片头。导向叶片头朝向转子103并且固定于定子143的固定环140上。
图4所示为沿着长轴121方向伸展的涡轮机的转动叶片120或导向叶片130的透视图。
涡轮机可以是飞机或机动车的用以产生电的燃气涡轮机，蒸汽涡轮机或压缩机。
叶片120、130沿着纵轴121方向具有相继排列的固定区域400，邻接于其的叶片平台403以及叶片面406和叶片顶415。
作为导向叶片130，叶片130可以在其叶片顶415上具有另一平台(未示出)。
在固定区域400内构造用以将转动叶片120、130固定于轴或盘上(未示出)的叶片根183。
叶片根183设计成例如锤头的形状。其他的圣诞树或燕尾榫脚形也是可行的。
叶片120、130对于流经叶片面406的介质具有一个流入边409和流出边412。
对于传统的叶片120，130，在叶片120，130的所有区域400，403，406内都可采用例如实心金属材料，特别是超合金。
这类超合金公开于例如EP1204776B1，EP1306454，EP1319729A1，WO99/67435或WO00/44949中；这些文献有关合金化学组成的内容是本发明公开的一部分。
叶片120，130在此可以通过浇铸法，也就是借助于取向凝结过程，通过锻造法，通过铣切法或它们的组合来制造。
将具有单晶结构的工件用作在工作时要耐受高机械、热和/或化学载荷的机械的零件。
通过诸如由熔体取向凝固的过程可制得这类单晶工件。这里所指的是一种浇铸法，该方法中液态的金属合金会凝固成单晶结构，即凝固成单晶的工件，或取向凝固。
并且，树枝状晶体沿着热流方向取向并构成棒状结晶晶粒结构(柱形，也即那些在工件的整个长度上分布的晶粒并且在此按照一般的语言习惯也称作为是取向凝固)或者构成单晶结构，即整个工件由单晶构成。在这些方法中，必需要避免转变为球晶(多晶)凝固，因为非取向的生长必然会形成横向和径向的晶粒边界，而这会使得取向凝固的或单晶的零件的良好性能失效。
一般在谈及取向凝固的结构时，指的既是不具有晶粒边界或顶多具有小角度晶粒边界的单晶，也指的是具有可能在径向上伸展的晶粒边界但没有横向的晶粒边界的棒状晶体结构。对于该第二种所述的晶体结构，也可称之为取向凝固的结构(方向性固化的结构)。
这些方法公开于US-PS6024792和EP0892090A1中；这些文献有关凝固方法的内容也是本申请公开的一部分。
同样，叶片120，130也可以具有耐受腐蚀或氧化的涂层，例如(McrAlX；M是铁(Fe)、钴(Co)、镍(Ni)这一组中的至少一个元素，X是活性元素并且表示钇(Y)和/或硅和/或稀土元素的至少一种，或铪(Hf))。这些合金公开于EP0486489B1、EP0786017B1、EP0412397B1或EP1306454A1，它们有关合金化学组成的内容也是本发明公开的一部分。
密度优选为理论密度值的95％。
在McrAlX-层(作为中间层或作为最外层)上形成有一个防护性的氧化铝层(TGO＝热生长氧化物层)。
在MCrAlX上还可以存在一个绝热层，该层优选是最外层并且由本发明的层体系1组成。
绝热层覆盖整个MCrAlX层。通过合适的涂覆方法，如电子辐射蒸发法(EB-PVD)而制得在绝热层中的棒状晶粒。
其他涂覆方法也是可以考虑的，例如气体等离子喷注法(APS)、LPPS、VPS或CVD。绝热层可以具有多孔的、带有微裂缝或大裂缝的晶粒以改善耐热冲击性。绝热层优选比MCrAlX层更多孔。
叶片120，130可以设计为空心或实心的。若要将叶片120、130冷却，则其是空心的并且任选还具有膜冷却孔418(虚线所示)。
图5所示为燃气涡轮机100的燃烧室110。燃烧室110设计成例如所谓的环形燃烧室的形状，其中许多在圆周方向上围绕旋转轴102排列的燃烧器107衔接入产生火焰156的公共燃烧室内腔154中。为此，在总体上将燃烧室110构造成围绕着旋转轴102排列的环形结构。
为了获得较高的效率，将燃烧室110设计用于约1000℃至1600℃的较高的工作介质M的温度。为了能够在不利于材料的操作参数下也能得到较长的操作持续时间，就要在燃烧室壁153的朝向工作介质M的那一侧设置由耐热护壳元件155构成的内衬。
由于在燃烧室110内部有着很高的温度，所以还能针对耐热护壳元件155或针对其支撑元件设置一个冷却系统。耐热护壳元件155是例如空心的并且还可任选地具有衔接于燃烧室内腔154内的冷却孔(未示出)。
每个合金制的耐热护壳元件155在工作介质一侧都设置有特别耐热的防护层(McrAlX-层和/或陶瓷层)或者由耐高温的材料(实心陶瓷石材)制成。
这些防护层可以类似于涡轮机叶片，也即例如MCrAlX：M是铁(Fe)、钴(Co)、镍(Ni)这一组中的至少一种元素，X为活性元素并且表示钇(Y)和/或硅和/或稀土金属中至少一种元素，或铪(Hf)。这类合金公开于EP0486489B1、EP0786017B1、EP0412397B1或EP1306454A1，它们有关合金的化学组成方面的内容也应是本申请公开的一部分。
在MCrAlX上还可例如有陶瓷绝热层，其由本发明的层体系1构成。
通过合适的涂覆方法，如电子辐射蒸发法(EB-PVD)而制得在绝热层中的棒状晶粒。
其他涂覆方法也是可以考虑的，例如气体等离子喷注法(APS)、LPPS、VPS或CVD。绝热层可以具有多孔的、带有微裂缝或大裂缝的晶粒以改善耐热冲击性。
再加工(再磨光)意味着，涡轮叶片120，130，耐热护壳元件155在其使用之后在适当情况下必须去除防护层(例如通过喷砂)。然后再去除腐蚀层和/或氧化层或产品。
任选地也要再修复涡轮机叶片120，130或者耐热护壳元件155中的裂缝。然后，再次涂覆涡轮叶片120，130，耐热护壳元件155并重新使用涡轮叶片120，130或耐热护壳元件155。

Claims (32)

1.陶瓷粉末，其由混晶烧绿石结构Gdv(ZrxHfy)Oz，其中v≈2，x+y≈2，z≈7，和含量为0.5wt％至10wt％的锆(Zr)和/或铪(Hf)的二次氧化物和任选地烧结助剂构成，所述烧结助剂为：
不超过0.05wt％的氧化硅
不超过0.1wt％的氧化钙
不超过0.1wt％的氧化镁
不超过0.1wt％的氧化铁
不超过0.1wt％的氧化铝，和
不超过0.08wt％氧化钛。
2.权利要求1所述的陶瓷粉末，其只具有氧化铪作为二次氧化物。
3.权利要求1所述的陶瓷粉末，其只具有氧化锆作为二次氧化物。
4.权利要求1所述的陶瓷粉末，其具有氧化锆和氧化铪作为二次氧化物。
5.权利要求1、2、3或4所述的陶瓷粉末，其中一种或多种二次氧化物只作为氧化物形式存在。
6.权利要求1、2、3或4所述的陶瓷粉末，
其具有最大3wt％的二次氧化物。
7.权利要求1、2、3或4所述的陶瓷粉末，
其具有最大8wt％的二次氧化物。
8.权利要求1所述的陶瓷粉末，其中，陶瓷粉末中的烧绿石相包括Gdv(ZrxHfy)Oz，其中x+y＝2，v＝2，z＝7。
9.权利要求1所述的陶瓷粉末，其中，陶瓷粉末中的烧绿石相包括Gd2(ZrxHfy)Oz，其中x+y≈2，z≈7。
10.权利要求1或9所述的陶瓷粉末，其中，陶瓷粉末中的烧绿石相包括Gdv(ZrxHfy)O7，其中v≈2，x+y≈2。
11.权利要求1、8或9所述的陶瓷粉末，其中，烧绿石相中铪与锆的混合比y∶x为30∶70至40∶60。
12.权利要求1、8或9所述的陶瓷粉末，其中，烧绿石相中铪与锆的混合比y∶x为50∶50。
13.权利要求1、8或9所述的陶瓷粉末，其中，铪与锆的混合比y∶X为60∶40至70∶30。
14.权利要求1、8或9所述的陶瓷粉末，其中，铪与锆的混合比y∶x为10∶90至20∶80。
15.权利要求1、8或9所述的陶瓷粉末，其中，烧绿石相中铪与锆的混合比y∶x为80∶20至90∶10。
16.权利要求1、8或9所述的陶瓷粉末，其中，y＞x。
17.权利要求1、8或9所述的陶瓷粉末，其中，y＜x。
18.由前述权利要求中一项或多项所述的粉末制得的外陶瓷层(13)。
19.层体系，其具有权利要求18所述的外陶瓷层(13)，该外陶瓷层(13)为最外层。
20.权利要求19所述的层体系，其中，在外陶瓷层(13)之下存在内陶瓷层(10)。
21.权利要求20所述的层体系，其中，内陶瓷层(10)由6wt％-8wt％钇稳定化的氧化锆层构成。
22.权利要求20或21所述的层体系，其中，内陶瓷层(10)的层厚为内陶瓷层(10)和外陶瓷层(13)的总层厚(D)的10％至40％。
23.权利要求20或21所述的层体系，其中，内陶瓷层(10)与外陶瓷层(13)的层厚总和为至少300μm。
24.权利要求20或21所述的层体系，其中，内陶瓷层(10)与外陶瓷层(13)的层厚总和为至少450μm。
25.权利要求19或20所述的层体系，其中，在基材(4)上和在内陶瓷层(10)下或在外陶瓷层(13)下存在金属结合层(7)。
26.权利要求25所述的层体系，其中，金属结合层(7)组成如下，wt％：
11％-13％的钴，
20％-22％的铬，
10.5％-11.5％的铝，
0.3％-0.5％的钇，
1.5％-2.5％的铼，和
余量的镍。
27.权利要求25所述的层体系，其中，金属结合层(7)组成如下，wt％：
24％-26％的钴，
16％-18％的铬，
9.5％-11％的铝，
0.3％-0.5％的钇，
1％-1.8％的铼，和
余量的镍。
28.权利要求20或21所述的层体系，其中，内陶瓷层(10)的层厚度为内陶瓷层(10)和外陶瓷层(13)的总层厚的50％至90％。
29.权利要求20或21所述的层体系，其中，内陶瓷层(10)的层厚度为内陶瓷层(10)和外陶瓷层(13)的总层厚的70％至90％。
30.权利要求20或21所述的层体系，其中，内陶瓷层(10)的层厚度为内陶瓷层(10)和外陶瓷层(13)的总层厚的60％至80％。
31.权利要求25所述的层体系，其由基材(4)、金属结合层(7)、内陶瓷层(10)和外陶瓷层(13)构成。
32.权利要求25所述的层体系，其由基材(4)、金属结合层(7)、金属结合层(7)上的氧化物层、内陶瓷层(10)和外陶瓷层(13)构成。
CN2008100956556A 2007-05-07 2008-05-07 具有钆-混晶-烧绿石相和氧化物的陶瓷粉末,陶瓷层和层体系 Expired - Fee Related CN101302103B (zh)

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