CN1868973A - 硅基衬底的涂层系统 - Google Patents

硅基衬底的涂层系统 Download PDF

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CN1868973A
CN1868973A CNA2006100682523A CN200610068252A CN1868973A CN 1868973 A CN1868973 A CN 1868973A CN A2006100682523 A CNA2006100682523 A CN A2006100682523A CN 200610068252 A CN200610068252 A CN 200610068252A CN 1868973 A CN1868973 A CN 1868973A
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T·巴蒂亚
W·R·施密德特
W·K·特雷维
V·R·韦杜拉
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Raytheon Technologies Corp
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Abstract

本发明提供了用于硅基衬底的粘合层系统，其中在所述硅基衬底和含硅金属的吸氧层之间提供了弹性模量为30－130GPa的柔性层。

Description

硅基衬底的涂层系统
美国政府权利
本发明得到了美国政府支持，由美国海军部提供资金，合同号为N-00014-03-C-0477。美国政府可以拥有本发明的某些权利。
技术领域
本发明涉及施加到含硅衬底上的粘合层(bond coat)系统。
背景技术
硅基单片陶瓷，比如碳化硅和氮化硅，以及复合材料，比如碳化硅纤维强化的碳化硅基质，由于具有高温机械和物理性质以及比金属低的密度，所以对于在燃气轮发动机热区中使用而言是有吸引力的材料。但是，这些材料在高温含水环境下，比如例如燃气轮发动机的燃烧室区和气轮机区，出现了加速氧化和退化。为了降低在这种环境中用作陶瓷部件的衬底在高温下的氧化和退化速率，在提供保护硅基衬底的阻挡层上已经给予了相当的努力，以提高这些部件的使用寿命。
图1a给出了构成现有技术的经过保护涂覆的陶瓷制品的一个变体。复合制品10包括硅基衬底12、包括致密连续硅金属层的粘合层或层14、和包括阻挡层16的环境阻挡涂层，所述阻挡层16包括基于钡和/或锶的碱土铝硅酸盐，或者硅酸钇。在所述阻挡层16的顶部，可以采用另一耐火顶层18，比如，例如，氧化铝、或者氧化锆、或者氧化钇或者其组合。图1b示出了现有技术的另一实施方案，其中包括了中间层20和22，从而赋予所述涂层系统柔性和/或化学相容性。所述中间层包括，例如，所述阻挡层材料和另外的氧化物比如莫来石的混合物。这些现有技术涂层系统已经证实具有相当的粘合性和保护性，而且已经用于防止硅基衬底12的退化和氧化。但是，现在已经发现，当现有技术所述的涂层施加到一些含硅衬底比如氮化硅上时，它们的机械性能受损，这通过抗弯强度或抗拉强度的降低得到了证实。相信机械性能的损失是源于粘合层14和含硅衬底12之间的机械不相容性。已经发现在粘合层14和含硅衬底12之间的弹性模量和热膨胀系数之间的不匹配，导致当所涂覆的系统10承受热偏差，比如从退火温度冷却和/或在燃气轮发动机操作过程中的加热和冷却循环时，粘合层14和含硅衬底12中产生热应变。还发现在这种系统中所储存的裂纹扩展所需的弹性应变能会很高。进一步发现，由于系统中的高应变和应力和/或高的弹性存储能，涂层系统和脆性陶瓷可能失效。由于硅粘合层和含硅衬底的脆性本质，热应变和最终的热应力可能导致在粘合层或衬底中出现开裂，或者导致粘合层和衬底之间的界面脱层。热应力高也可以导致出现局部应力集中并激活所述粘合层或含硅衬底中的小瑕疵或缺陷，从而导致在远远低于典型衬底典型强度下失效。
基于上述内容，显然仍需要针对硅基陶瓷衬底的改进粘合层系统，它不会对衬底的机械行为产生负面影响，比如降低抗弯强度或抗拉强度。所以，本发明的主要目标是提供这种涂层系统结构。
相应地，本发明的主要目标是提供不会对硅基衬底比如氮化硅的机械性能有负面影响的粘合层系统。本发明的粘合层系统结合了含硅金属的粘合层以及施加其上的阻挡涂层所提供的优点，并同时克服了上述缺点。
发明内容
通过本发明实现了上述目标，其中在硅基衬底和吸氧层之间提供了弹性模量为30-130Gpa的柔性层(compliant layer)。在本发明中，通过在吸氧层和衬底之间提供柔性层使涂层系统具有更大的缺陷容忍度，从而缓解了衬底强度的下降。因此，所述涂层系统保留了现有技术系统的优点，同时不损失衬底强度。所述对强度损失的缓解源于本发明的涂层设计，它包括柔性层、吸氧层和另外的阻挡层，降低了和衬底相邻的层中的残余拉伸应力和/或减少了涂层系统储存的弹性应变能。而且，所述柔性层起到对衬底中的应力集中进行缓冲的作用，因而有助于保持衬底强度。本发明的粘合层系统和目前所知的现有技术相比具有明显的提高。
下面将给出本发明的进一步目标和优点。
附图说明
图1a和1b是根据现有技术的复合制品的示意图；
图2是根据本发明一个实施方案的复合制品的示意图；和
图3给出了本发明在保留涂覆制品强度方面的优点。
具体实施方式
参见图2，示出了本发明的复合制品100，它包括硅基衬底120、吸氧层140、和位于所述硅基衬底和所述含硅金属的吸氧层之间的柔性层30。应该注意到，现有金属中的粘合层材料大多数是吸氧剂，比如硅(Si)和耐火金属硅化物和其组合。尽管含硅吸氧层140是本发明的优选实施方案，但是可替换地，层140也可以是现有技术公知的氧化铝或氧化铬形成体的高温金属合金。
根据本发明，柔性层30选自碱土铝硅酸盐、单硅酸钇、二硅酸钇、稀土单硅酸盐和二硅酸盐、硅酸铪、硅酸锆；铪、锆、钇、稀土金属、铌、钛、钽、硅、铝的氧化物；氮化硅；碳化硅；氧氮化硅；氧碳化硅；氧碳氮化硅；硅耐火金属氧化物；形成氧化铝的耐火金属合金；形成氧化铬的耐火金属合金，和其混合物。优选柔性层的组成选自氧化钇、氧化铪、稀土金属氧化物、单硅酸钇、二硅酸钇、稀土单硅酸盐和二硅酸盐、硅酸铪、和其混合物。柔性层的优选弹性模量是30-130GPa。为了确保上述的所需行为性质，必须控制柔性层的孔隙率。优选柔性层的孔隙率为约2-50％，更优选为约5-25％。孔隙率是指柔性层30中的空隙分数。柔性层的厚度优选为20-250μm，更优选为40-125μm。柔性层和吸氧层的厚度比优选是0.1∶1-10∶1。柔性层30可以包括具有上述材料组成的多层。如果需要，柔性层30和吸氧层140可以在环境阻挡涂层系统中重复一次或多次。
硅基衬底120包括选自单片氮化硅、单片碳化硅、含氮化硅的复合材料、含碳化硅的复合材料、氧氮化硅、氧碳化硅、碳氮化硅、含硅的钼合金、含硅的铌合金材料。
本发明的制品还包括在所述粘合层系统上施加的环境阻挡层160和180。所述阻挡层提供了在高温和高压下的抗高速蒸气的保护。所述阻挡层可以包括莫来石，包括钡锶铝硅酸盐(BSAS)和锶铝硅酸盐(SAS)的碱土铝硅酸盐，硅酸钇，稀土硅酸盐，铪或锆硅酸盐，铪、锆、钛、硅、钇、稀土金属、钽、铌、铝的氧化物，和其混合物。
上述层可以通过现有技术所知的任何加工方法施加，包括热喷涂、化学气相沉积、物理气相沉积、电泳沉积、静电沉积、先驱体热解(preceramic polymer pyrolysis)、溶胶-凝胶、浆料涂覆、浸提、气刷(air-brushing)、溅射、浆料涂漆或其任何组合。为了在柔性层中获得所需孔隙率，可以采用牺牲性成孔剂在柔性层中产生孔隙率。牺牲性成孔剂是本领域公知的，包括材料比如聚酯、聚苯乙烯等。
通过采用本发明的粘合层系统，其中采用了弹性模量为30-130GPa的柔性层并结合吸氧层，缓解了裂纹形成和/或裂纹从涂层到衬底或者反之的扩展。从而使得涂覆的衬底的保留强度接近基础衬底的强度，这对于结构应用非常重要。涂3示出了具有所述新的环境阻挡涂层(EBC)粘合层结构的SN282氮化硅的四点弯曲强度，以保留强度和SN282材料(没有EBC)基准强度相比的分数形式给出。图中示出了新的粘合层结构的两种不同变体。未涂覆的SN282的基准强度范围用阴影表示。虚线表示采用硅直接施加到氮化硅衬底上的现有技术EBC结构所保留的一般强度分数。下面的实施例描述将进一步验证所述新EBC结构的优点。
实施例1
在具有2.5重量％Darvan的10ml去离子水(100ml水中有2.5gm的Darvan)中，加入26.67gm的二硅酸钇(Y2Si2O7)。浆料球磨30分钟。将六根氮化硅条浸入浆料中并干燥。随后，所涂覆的条在1350℃烧制5小时。重复一次所述浸入工艺，将条在1350℃重新烧制5小时。随后，将试样放入CVD反应器中，涂覆35和70μm的硅。反应器维持在850-900℃，经由下面的反应沉积硅：
涂覆试样的抗弯强度采用四点弯曲法测量，发现平均强度和未涂覆的氮化硅试样具有可比性(图3)。从图3可以发现，未涂覆的氮化硅即使在涂覆后，也维持了高强度。
实施例2
在具有2.5重量％Darvan的10ml水(100ml水中有2.5gm的Darvan)中，加入31.33gm的单硅酸钇(Y2SiO5)。浆料球磨30分钟。将六根氮化硅条浸入浆料中并干燥。随后，所涂覆的条在1350℃烧制5小时。重复一次所述浸入工艺，将条在1350℃重新烧制5小时。随后，将试样放入CVD反应器中，涂覆20μm的硅。反应器维持在850-900℃，经由下面的反应沉积硅：
涂覆试样的抗弯强度采用四点弯曲法测量，发现平均强度是未涂覆的氮化硅条的90％。
实施例3
采用空气等离子喷涂在氮化硅衬底上沉积125μm的硅。涂覆条的抗弯强度采用四点弯曲法测量，发现平均强度是未涂覆的氮化硅条的大约50％。
可以理解本发明不限于本文所述和所示的举例说明，应该认为其仅仅是举例说明本发明的最佳实施方式，而且可以对部件的形式、尺寸和排列以及操作细节进行修改。本发明更意在包括落在权利要求所限定的精神和范围中的所有这种修改。

Claims (17)

1、一种制品，包括：
硅基衬底；
吸氧层；
位于所述硅基衬底和吸氧层之间的柔性层，其中所述柔性层具有30-130GPa的弹性模量；和
在所述吸氧层上的环境阻挡涂层(EBC)。
2、权利要求1的制品，其中所述柔性层选自碱土铝硅酸盐、单硅酸钇、二硅酸钇、稀土单硅酸盐和二硅酸盐、硅酸铪、硅酸锆；铪、锆、钇、稀土金属、铌、钛、钽、硅、铝的氧化物；氮化硅；碳化硅；氧氮化硅；氧碳化硅；氧碳氮化硅；硅耐火金属氧化物；形成氧化铝的耐火金属合金；形成氧化铬的耐火金属合金，和其混合物。
3、权利要求2的制品，其中所述柔性层具有约2-50％的孔隙率。
4、权利要求2的制品，其中所述柔性层具有约5-25％的孔隙率。
5、权利要求2的制品，其中所述柔性层具有20-250μm的厚度。
6、权利要求2的制品，其中所述柔性层具有40-125μm的厚度。
7、权利要求1的制品，其中所述柔性层和吸氧层具有约0.1∶1-10∶1的柔性层对吸氧层的厚度比。
8、权利要求2的制品，其中所述柔性层选自氧化钇、氧化铪、稀土金属氧化物、单硅酸钇、二硅酸钇、稀土单硅酸盐和二硅酸盐、硅酸铪和其混合物。
9、权利要求1的制品，其中所述硅基衬底选自单片氮化硅、单片碳化硅、含氮化硅的复合材料、含碳化硅的复合材料、氧氮化硅、碳氮化硅、氧碳化硅、含硅的钼合金、含硅的铌合金。
10、权利要求1的制品，其中所述EBC包括选自莫来石、碱土铝硅酸盐、钡锶铝硅酸盐、硅酸钇、稀土硅酸盐、氧化铪、氧化锆、氧化钛、氧化硅、氧化钇、稀土金属氧化物、氧化钽、氧化铌、氧化铝和其混合物的至少一层。
11、权利要求10的制品，其中所述EBC包括多层。
12、权利要求1的制品，其中所述吸氧层选自硅金属、硅金属合金、金属间硅化物、形成氧化铬的金属合金、形成氧化铝的金属合金和其混合物。
13、权利要求1的制品，其中所述柔性层和吸氧层至少重复一次。
14、权利要求1的制品，其中所述EBC涂层位于基本全部所述吸氧层上。
15、一种制品，其包括包括涂覆的硅基衬底、吸氧层以及位于之间的柔性层的复合材料，所述柔性层保留了其初始衬底强度的约70％，更优选90％和以上。
16、一种制备权利要求1的制品的方法，其中所述柔性层、吸氧层和EBC的至少之一采用热喷涂、化学气相沉积、物理气相沉积、电泳沉积、静电沉积、先驱体热解、溶胶-凝胶、浆料涂覆、浸提、气刷、溅射、浆料涂漆或其任何组合沉积。
17、一种制备权利要求1的制品的方法，其中所述至少一种牺牲性成孔剂被用来控制所述柔性层的孔隙率以及由此控制其模量。
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