CN107074671B - 耐环境性被膜 - Google Patents
耐环境性被膜 Download PDFInfo
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Abstract
在水蒸气氧化性气氛下利用的被膜具备包含赛隆的第1层、以及包含莫来石的第2层,所述第2层被覆前述第1层并被暴露于前述气氛,前述第1层与前述第2层相互相接,以此被覆母材。
Description
技术领域
本公开涉及将航空器的发动机等进行被覆的被膜,特别涉及在高温且氧化性环境中保护发动机等的被膜。
背景技术
改善航空器发动机的包含燃料效率在内的诸性能,是一直持续要求的技术课题。如人们熟知的那样,改善燃料效率的重要的关键因素是轻型化,但可以与其并列地举出运行温度的提高。如果在更高温度下运行发动机则热效率得以改善,以此可期待改善燃料效率。
以往以来,人们利用镍基超合金作为耐热材料,但为了实现更进一步的轻型化以及耐热性提高,因而正在研究陶瓷基复合材料(CMC)的利用。CMC例如是通过将由碳化硅(SiC)纤维形成的织物与由SiC形成的基体进行复合化而得到的材料(SiC/SiC)。此外,可以有C/C、C/SiC、SiC/Si3N4、Al2O3/Al2O3等各种组合。
SiC具有极其高的耐热性,另外在氧化后生成的二氧化硅(SiO2)可以保护SiC以防止被进一步氧化。然而,发动机所吸入的空气中包含有不能忽视的量的水蒸气。该水蒸气在高温下与二氧化硅进行反应而使其变成挥发性的氢氧化物,因而最终不能防止SiC的损耗。为了防止这样的高温水蒸气氧化,提出了利用耐环境性被膜(EBC)来被覆CMC的技术。专利文献1、2中公开了相关的技术。
现有技术文献
专利文献
专利文献1:美国专利申请公开2003/0003328A1
专利文献2:日本国专利申请公开H11-12050号
发明内容
发明想要解决的课题
莫来石(mullite:典型地是由3Al2O3·2SiO2表示的硅酸铝)在高温氧化性气氛下也稳定,是在保护母材的被膜中常常利用的物质。然而,根据本发明人等的研究,为了接近实用的条件而置于反复设为常温气氛与高温气氛的循环条件下时,观察到莫来石被膜的耐环境性能常常会发生劣化。很难认为其主要原因可以归因于因所谓热冲击而导致在被膜中产生缺陷。这是因为,即使使缓和莫来石与母材之间的热膨胀系数(thermal expansioncoefficient)的差的层介入,也不能充分防止该劣化。
用于解决问题的方案
本发明人等查明了该问题的原因,以此想到了以下公开内容所涉及的被膜。
根据一方面,在水蒸气氧化性气氛下利用的被膜具备包含赛隆(sialon)的第1层、以及包含莫来石的第2层,所述第2层被覆前述第1层并被暴露于前述气氛,前述第1层与前述第2层相互相接。
发明的效果
被膜即使被反复放置于常温气氛与高温气氛中也能够持续维持耐环境性能。
附图说明
图1为本实施方式的被膜的概念性的截面图。
图2为在水蒸气氧化性的气氛中放置的被膜的概念性的截面图。
具体实施方式
参照附图在以下说明几个实施方式。
本发明涉及的被膜,可以在例如超过1100℃的高温且是氧化性的气氛下,用作保护母材不受环境损害的耐环境性被膜,特别是在包含水蒸气的高温气氛下,可以出于保护SiC/SiC等CMC不受环境损害的目的而适宜利用,但未必受限于此。
参照图1,耐热材料1包含母材11、覆盖母材11的第1层13、以及被覆第1层13并被暴露于气氛中的第2层15。母材11例如是由包含SiC/SiC的CMC形成的耐热材料。
第1层13包含赛隆,或者由赛隆形成。赛隆通常是可理解为氮化硅(Si3N4)与氧化铝(Al2O3)的固溶体的陶瓷。由于氮化硅结晶存在多个形态(例如α-Si3N4以及β-Si3N4),因而赛隆的结晶也具有多个形态,其中β’-赛隆是高熔点且在有问题的温度区域中不引起相转变,从这个观点考虑,适合于本实施方式。或者也可以包含O’-赛隆、X-赛隆、或者如氧化铝那样的其它的相。为了享受铝离子的供给能力,其它的相越少越有利。因此,其它的相相对于赛隆小于50体积%,优选小于30体积%,更优选小于10体积%。
第1层13介于母材11与第2层15之间。优选的是,第1层13与母材11直接相接而与其结合,但是也可以出于提高密合性、其它目的而使其它的层介入。另外优选的是,第1层13实质上整面地由第2层15被覆,不暴露于氧化性气氛。另外优选的是,第1层13与第2层15直接相接而相互结合,但是如后述那样,其它的相可以以极薄的层的形态或其它的形态介于第1层13与第2层15之间。
第2层15包含莫来石,或者由莫来石形成。如已叙述的那样,莫来石典型地是由3Al2O3·2SiO2表示的硅酸铝。或者莫来石也可以从该化学计量组成偏离。
第2层15可以包含其它的相,例如可以包含Re2Si2O7的相,其中,Re是Y、Yb、Er、Dy中的任1个以上。为了享受基于莫来石的保护能力,其它的相越少越有利。因此,其它的相相对于莫来石小于50体积%,优选小于30体积%,更优选小于10体积%。
如上所述,第2层15将第1层13被覆并自身被暴露于气氛中。第2层15通常直接露出于气氛中。或者,也可以其它的层进一步部分地或者整面地被覆第2层15。关于该其它的层,以防止外来物质的附着等为目的,可以是在使用一定时间之后会损耗那样的性质。
关于各层,越厚则越提高耐环境性,但如果过厚则容易发生如裂纹那样的缺陷。因此各层例如为5~300μm的范围,或者为10~100μm的范围。虽然在第1层13上层叠第2层15,但也可以进一步层叠多个这样的组合而形成多层。
参照图2,当具备本实施方式的被膜的耐热材料1放置于高温氧化性气氛时,氧离子(O2-)在暴露于气氛的第2层15的表面变得丰富,作为结果,在第2层15内产生氧离子(O2-)从表面朝向下层递减的浓度梯度。为了与其平衡,铝离子(Al3+)发生如箭头D那样朝向表面扩散的倾向,即,产生与氧离子相反方向的浓度梯度。
如果没有赛隆,则在第2层15,特别是在其底部,发生铝离子相对缺乏而导致莫来石变得不稳定的倾向。如果莫来石分解,则生成如方石英那样的二氧化硅,这是伴随体积变化的分解反应。另外,方石英也是多种形态,在约270℃时,在β相(高温相)与α相(低温相)之间引起相转变,这也是伴随体积变化。
这些体积变化是损害莫来石层的密合性、或者在莫来石层内生成如裂纹那样的缺陷的原因。特别是在实用条件下,被膜反复被暴露于常温气氛与高温气氛,反复发生上述的相转变,因而不能忽视密合性的劣化或缺陷的产生。剥离或缺陷的产生必然带来耐环境性能的降低。
在本实施方式中,由于如箭头S那样从第1层13供给铝离子,因而可以防止莫来石的分解。随着供给,第1层13将失去一部分的铝离子,但这只不过会使赛隆中的Si3N4与Al2O3之间的固溶比发生变化,通常不伴随结晶形的变化。即,对于在第1层13以及第2层15中的任一层都不用担心发生引发问题的体积变化。
附带说,莫来石中的铝离子的向外扩散、以及因其而导致的莫来石的分解使得被膜发生劣化,是本发明人等的发现,与赛隆的组合因发现该问题的原因而想到了。
如根据上述说明而理解的那样,为了通过供给铝离子来防止莫来石的分解,优选在第1层13与第2层15之间没有针对其扩散的屏障。因此如已叙述的那样,优选第1层13与第2层15直接相接而相互结合。但是,在允许铝离子扩散的限度,也可以使其它的相介入,即使那样也可视为实质上相互相接的形态。作为这样的形态,例如是极薄的层的形态,但是也可以是分散在界面附近的颗粒状的形态、其它的形态。以层的形态介入的情况下,可认为例如小于1μm是限度。
如果第1层13相对于第2层15而言过薄,则供给铝离子的能力不足,如果与其相反,那么基于第2层15的保护能力很有可能不足。因此,第1层13的厚度与第2层15的厚度相比,优选为0.1~2.0的范围,更优选为0.2~1.0。
如已叙述的那样,赛隆是Si3N4与Al2O3的固溶体,但是β’相并非在任意的比例下稳定。由Si6-zAlzOzN8-z这样的通式表示时,若z超过4.2,则β’相作为单相并不稳定,例如需要Al2O3相的共存。如果因铝离子向外扩散而导致Al2O3相与β’-赛隆相的共存比例发生变动,则这很可能成为层中产生缺陷的原因。为了防止这个问题,有效的是在第1层13中赛隆成为β’相的单相,即,优选z为0<z≤4.2的范围。z越大则供给铝离子的能力越增大。因此更优选为1.0≤z,进一步优选为2.0≤z。另外,z越小则越不易析出Al2O3相。因此更优选为z≤3.5,进一步优选为z≤3.0。
如已叙述的那样,莫来石也可以从化学计量组成偏离。例如在由Al4+2xSi2-2xO10-x表示时,优选x为0.20≤x≤0.39的范围。从抑制铝离子扩散的观点考虑,进一步优选为0.20≤x≤0.34的范围,更优选为0.23≤x≤0.30的范围。另外,对于第2层15,也可以将相互不同组成的莫来石进行混合、或者层叠。
在第1层13与第2层15的任一方中、或者双方中,也可以具有组分梯度。例如对于第2层15,也可以使Al/Si比在朝向表面的方向上逐渐增大(在上述的化学式中x增大)。这有利于例如在表面抑制由水蒸气氧化导致的损耗,另外,有利于缓和相对于第1层13的热膨胀系数的差异。
如上所述的被膜可以通过任意的方法而形成。作为制造方法的例子,可列举气溶胶沉积、电子束蒸镀、激光化学蒸镀。
例如利用气溶胶沉积,可以如下操作而形成被膜。例如在形成第1层13时,将赛隆的(在形成第2层15时为莫来石的)粉末分散于如氮气、氩气、氦气、氧气、空气那样的载气中而制成气溶胶,将该气溶胶喷射在母材(或者第1层)上,从而形成被膜。也可以通过缓慢地改变供给的粉末的组成,从而形成梯度组分被膜。或者,通过一边继续形成被膜,一边将所供给的粉末由赛隆快速变更为莫来石,从而能够连续地进行第1层13的形成与第2层15的形成。也可以在形成被膜之后,接着组合实施将表面平滑化的处理、热处理。
为了验证本实施方式的效果,制作了如下那样的模拟性的层叠体。
作为莫来石粉末,采用了名称为KM-101(共立材料株式会社)的通常能够获取的粉末。将该粉末在19.6MPa下进行单轴加压,然后在冷间、245MPa下各向同性地进行加压,从而获得了圆柱形以及中空圆柱形的生坯。将该生坯分别在常压下在1300℃烧成50小时,接着进一步在1750℃烧成5小时,从而获得了15mm(外径)×5mm(高度)的圆柱形试样M1、以及15mm(外径)-2.1mm(内径)×0.2mm(高度)的中空圆柱形试样M2。
将纯度99.999999999%的硅锭(信越化学工业株式会社)加工为2mm(外径)×0.2mm(高度)的圆柱形,获得了硅试样。这是正好嵌入于试样M2的空洞的尺寸。
作为β’-赛隆粉末,采用了名称为BSI3-001B(AG Materials Inc.)的通常能够获取的粉末(在Si6-zAlzOzN8-z中z=3)。以19.6MPa对该粉末进行单轴加压,从而获得了圆柱形的生坯。将该生坯,在0.7MPa的氮气气氛下,在1750℃以40MPa进行热压2小时,从而获得了2mm(外径)×0.2mm(高度)的圆柱形的β’-赛隆试样。
将硅试样与β’-赛隆试样分别嵌入于试样M2的空洞中,将它们用一对试样M1从上下夹持。将该组装件在1600℃、在减压下,以50MPa供给于热压1小时,获得了接合体。通过仅对这些接合体的一面进行磨光研磨,减薄一方的莫来石层,以使得直到埋设的硅为止或直到β’-赛隆为止的厚度成为0.25mm。该减薄了的莫来石层模拟暴露于气氛的莫来石被膜。
将这些莫来石/硅接合体以及莫来石/β’-赛隆接合体在1400℃加热10小时,将加热后的接合体纵向切断并进行研磨,通过SEM观察纵截面。
在莫来石/硅接合体的减薄了的莫来石层中,在与硅层的界面附近,观察到能够与莫来石相区分的粒状组织。在没有减薄的莫来石层中,在界面附近也没有发现与此同样的组织。即,可认为粒状组织是在暴露于气氛时所特有的组织。
在与上述相同的视野中,进行了EDS元素映射,结果是发现了Al、Si、O的分布的不均匀,且发现了该不均匀对应于粒状的结构。即,暗示在粒状的结构是莫来石发生分解而生成了二氧化硅,可认为如果没有赛隆层则存在莫来石在莫来石层的底部发生分解的倾向。
在莫来石/β’-赛隆接合体方面,即使在加热后,也没有观察到如上所述的粒状组织。在EDS元素图中Al、Si、O的分布也是均匀的。即,可确认通过使莫来石层与β’-赛隆层相接从而可以防止莫来石的分解。
根据以上的试验结果,可认为如果在被膜中,包含赛隆的第1层与包含莫来石的第2层相互相接,则被膜持续维持耐环境性能。
虽然说明了几个实施方式,但具有本技术领域的通常技术的人员基于上述公开内容能够对实施方式进行修改或变形。
产业上的可利用性
提供一种即使反复放置于常温气氛与高温气氛下也持续维持耐环境性能的被膜。
Claims (4)
1.一种被膜,其是在水蒸气氧化性气氛下利用的被覆陶瓷基复合材料的被膜,具备包含赛隆的第1层、以及包含莫来石和Re2Si2O7相的第2层,
所述第2层被覆所述第1层并被暴露于所述气氛,
所述第1层与所述第2层相互相接,
其中,Re是Y、Yb、Er、Dy中的任1种以上,所述Re2Si2O7相相对于莫来石小于50体积%。
2.根据权利要求1所述的被膜,其中,所述赛隆为β’型。
3.根据权利要求1或2所述的被膜,其中,所述第2层为5~300μm的厚度。
4.根据权利要求1或2所述的被膜,其中,所述第1层为5~300μm的厚度,结合于所述陶瓷基复合材料而进行被覆。
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