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CN113825857A - 在金属基材表面形成氧化铝层的方法 - Google Patents

在金属基材表面形成氧化铝层的方法 Download PDF

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Publication number
CN113825857A
CN113825857A CN202080036200.6A CN202080036200A CN113825857A CN 113825857 A CN113825857 A CN 113825857A CN 202080036200 A CN202080036200 A CN 202080036200A CN 113825857 A CN113825857 A CN 113825857A
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layer
aluminium
substrate
metal substrate
halogen
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CN113825857B (zh
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M·C·卡瓦洛克
S·尼特尔
J·赛派赫
L·玛蒂努
F·博格隆
S·洛克埃
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Safran SA
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Safran SA
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Abstract

本发明涉及一种在包含铝的金属合金基材(201)的表面上形成氧化铝层(203)的方法，该方法至少包括：‑在金属基材的表面上沉积第一铝层，‑通过气相沉积在第一层上沉积第二层，该第二层包含铝、卤素和氧，以及‑在氧化气氛下对涂有第一层和第二层的基材进行热处理，以在金属基材的表面形成氧化铝层。

Description

在金属基材表面形成氧化铝层的方法
技术领域
本发明涉及一种在金属基材表面形成氧化铝层以赋予所述基材在高温下防止氧化和腐蚀的方法。本发明尤其涉及对旨在用于航空涡轮机中的基材的保护。
背景技术
在航空涡轮机中使用镍基超合金是已知的。为了减轻涡轮机的重量，已经开发了包含较轻金属(例如铝)的合金。例子包括基于铝化钛(也称为TiAl)的合金，其具有良好的机械特性，并且比镍基超合金轻得多。
然而，希望提高这些合金在高温下(即高于800℃的温度下)的抗氧化和抗腐蚀性能。已经开发出在这些类型的合金表面上形成氧化铝保护层的解决方案。特别是，Hornauer等人的出版物(表面和涂层技术(Surface and Coatings Technology),2003,174,第1182-1186页)提出了一种解决方案，其中首先通过等离子体工艺在部件的表面注入氯，然后在其中形成保护性氧化铝层。然而，这种解决方案的缺点是在形成氧化铝层的过程中导致零件表面附近的局部贫铝。这种贫铝可能导致基材在高温下的性能发生不希望的变化，尤其是由于易碎金属间相的形成，这会降低材料的疲劳寿命。
发明内容
本发明涉及一种在包含铝的金属合金基材的表面上形成氧化铝层的方法，该方法至少包括：
-在金属基材的表面上沉积第一铝层，
-通过气相沉积在第一层上沉积第二层，该第二层包含铝、卤素和氧，以及
-在氧化气氛下对涂有第一层和第二层的基材进行热处理，以在金属基材的表面形成氧化铝层。
本发明提出了一种解决方案，其中在沉积包含铝、卤素和氧的第二层之前，在基材上沉积铝中间层(第一层)。该第一层提供铝以在氧化气氛下热处理期间形成氧化铝层。由于该提供铝的操作，减少或甚至消除了现有技术中遇到的下层金属基材的局部贫铝现象。
在实施方式的一个示例中，第一层的厚度大于或等于20nm。
当形成氧化铝层时，这样的厚度值有利地使得可以进一步减少下层基材的贫铝现象。
在实施方式的一个示例中，第一层的厚度小于或等于1000nm，例如500nm。
限制第一层的厚度避免了铝不从第一层扩散到下层基材并在其中引起结构变化的任何风险。
特别地，第一层的厚度可以在20nm至1000nm之间，例如在20nm至500nm之间。
在实施方式的一个示例中，通过选自物理气相沉积、化学气相沉积、等离子体增强化学气相沉积和表面硬化等的方法来沉积第二层。
第二层包含式AlOnXm的化合物，其中n和m各自严格地为正数且X代表卤素。
特别地，第二层可以包含卤化铝和卤氧化铝的混合物，任选地包含氧化铝。
在实施方式的一个示例中，卤素是氟。在此情况下，第二层可以包含式AlOnFm的化合物，其中n和m各自严格地为正数。特别地，第二层可以包含氟化铝和氟氧化铝的混合物，任选地包含氧化铝。作为一个变化形式，卤素是氯。
在实施方式的一个示例中，第二层的厚度大于或等于10μm，优选地在10μm至50μm之间。这样的厚度一方面可以改善氧化铝层的生长，另一方面可以使层中的内应力最小化，这使得层能够避免与基材发生粘合缺陷的任何风险。
在实施方式的一个示例中，第二层由包含卤素气体、氧和铝的气相沉积。
例如，第二层由包含氟、氧和铝的气相沉积。当卤素是氟时，气相可包含CF4、C2F6、SiF4、SF6或这些化合物的混合物，以及氧和铝。
作为一个变化形式，第二层由包含氯、氧和铝的气相沉积。当卤素是氯时，气相可包含SiCl4、Cl2或这些化合物的混合物，以及氧和铝。
在实施方式的一个示例中，通过在包含氧(氧气)和卤素气体的气氛中对包含铝的靶进行溅射来沉积第二层。
在实施方式的一个示例中，热处理在高于或等于800℃的温度下进行。
在实施方式的一个示例中，金属基材是铝化钛基合金。
在实施方式的一个示例中，金属基材是涡轮机部件，例如航空涡轮机部件。
根据其另一方面，本发明还涉及一种经涂覆的金属基材，其包含：
-包含铝的金属合金基材，
-在金属基材表面上的第一铝层，和
-包含铝、卤素和氧的第二层，该第二层涂覆第一层。
上述经过涂覆的金属基材是在氧化气氛下进行上述方法热处理得到的中间产物。
在实施方式的一个示例中，第一层的厚度大于或等于20nm。第一层的厚度可以小于或等于1000nm，例如500nm。特别地，第一层的厚度可以在20nm至1000nm之间，例如在20nm至500nm之间。
在实施方式的一个示例中，第二层的卤素是氟。
特别地，第二层可以包含式AlOnFm的化合物，其中n和m各自严格地为正数。特别地，第二层可以包含氟化铝和氟氧化铝的混合物，任选地包含氧化铝。
附图说明
[图1]图1示出了在实施根据本发明方法的一个示例的第一步骤之后涂覆有第一铝层的基材。
[图2]图2示出了在实施根据本发明方法的一个示例的第二步骤之后涂覆有第一层和第二层的基材。
[图3]图3示出了在氧化气氛下热处理后获得的表面涂有氧化铝层的基材。
[图4]图4示意性地描述了可以在本发明的上下文中实施的用于将层气相沉积到基材上的装置。
[图5]图5示出了通过扫描电子显微镜得到的在实施根据本发明方法之后获得的结果的照片。
[图6]图6显示了通过扫描电子显微镜得到的在实施非本发明方法之后获得的结果的照片，其中未沉积第一铝层。
具体实施方式
本发明涉及包含铝的合金的金属合金基材11的涂层。处理过的基材可以是铝化钛基合金，例如γ-TiAl合金。
处理过的基材可以构成涡轮机部件，例如航空涡轮机部件。基材旨在用于氧化气氛中以及高于或等于800℃的温度下。例如，基材可以是涡轮机部件。例如，其可以是涡轮叶片或涡轮环扇区。
首先将第一铝层12沉积到基材的外表面S上。第一层12可以沉积为接触基材的外层S。可以通过实施本身已知的技术来沉积由元素铝(Al)形成的第一层12。特别地，其可以通过物理气相沉积来沉积，例如通过真空蒸发或通过溅射来进行。第一铝层12可以通过其他沉积方法沉积，例如电化学沉积、化学气相沉积(CVD)、等离子体增强化学气相沉积(PECVD)或表面硬化。沉积第一层12时施加的温度可以在20℃至600℃之间，例如在20℃至400℃之间。
在实施方式的一个示例中，例如，第一铝层12可以通过射频磁控溅射来沉积，该操作过程使用例如功率等于200W，在减压下、例如0.66巴下进行，使用氩气流，例如60标准立方厘米/分钟，温度为400℃。
第一层12可以具有在20nm至1000nm之间的厚度e1。
涂有第一层12的金属基材11如图1所示。
然后在第一层12上形成包含铝、卤素和氧的第二层13。第二层13可以沉积为与第一层12接触。第一层12介于基材11和第二层13之间。第二层13通过气相沉积形成。
如上所述，第二层13包含式AlOnXm的化合物，其中n和m各自严格地为正数且X代表卤素。第二层13可以包含卤化铝和卤氧化铝的混合物，任选地包含氧化铝。卤素可以是如上所述的氟或氯。
以原子百分比计，第二层13可以包含：
-3％至70％的卤素，例如55％至65％的卤素，
-5％至40％的铝，例如10％至30％的铝，以及
-1％至20％的氧，例如3％至15％的氧。
第二层13可以具有介于2:1和8:1之间的卤素和氧之间的原子比。
发明人已经观察到卤素是通过氧对铝的氧化形成氧化铝的反应的活化剂。
第二层13通过气相沉积制成，特别是通过磁控阴极溅射制成。沉积第二层13时施加的温度可以在20℃至800℃之间，例如在20℃至400℃之间。
图4示意性地显示了通过磁控阴极溅射进行沉积的装置。
在腔室101中，通过入口106引入气体并且在靶105和待涂覆的基材111之间产生等离子体。在通过在靶105和基材111之间施加电压而获得的电场的作用下，靶产生电子并且可以通过碰撞使构成等离子体的原子电离。由位于靶105附近的磁体104产生的磁场的存在将产生的电子限制在靶附近，并增加了电子与等离子体中原子在此发生碰撞的可能性。当发生这样的碰撞时，产生高能空间，该高能空间可以通过弹性冲击而轰击靶105并从靶105撕裂粒子。如此撕裂的靶105的粒子随后可沉积在基材111上，形成沉积物。
第二层13可以在真空下沉积，例如在小于或等于10Pa(75毫托)的压力下，例如在0.67Pa(5毫托)至10Pa(75毫托)之间的压力下进行。在沉积期间，可以施加以下条件：
-注入腔室101的氧气流速介于每分钟1标准立方厘米(sccm)和每分钟100标准立方厘米之间，并且
-腔室101中的卤素气体流速介于每分钟2.5标准立方厘米和每分钟100标准立方厘米之间，
-并且，任选地，注入腔室101的惰性气体流速介于每分钟1标准立方厘米和每分钟100标准立方厘米之间。
例如，惰性气体可以是氩气。
在卤素为氟的情况下，卤素气体可选自CF4、C2F6、SiF4、SF6或这些化合物的混合物。
在卤素为氯的情况下，卤素气体可选自SiCl4、Cl2或这些化合物的混合物。
第二层13可以具有大于或等于0.1μm，例如10μm，例如在10μm至100μm之间的厚度e2。
图2表示涂有第一铝层12和第二层13(例如，如上所述)的基材11。
然后，在氧化气氛下进行热处理，以在金属基材的表面S上形成氧化铝层14。
然后可以在高于或等于800℃，例如在800℃至1000℃之间，例如在850℃至900℃之间的温度下进行热处理。
热处理可以在空气中进行。热处理可以是退火。
如上所述，由于铝层12的存在，在热处理期间发生氧化铝层14的生长，同时限制或甚至消除了基板表面S附近的贫铝。
在热处理结束时，如图3示意性所示，在金属基材11的表面S处形成氧化铝层14。
热处理也可以在氧化铝层14上形成包含钛、铝和氧的层15时进行。
在实施方式的一个示例中，氧化铝层14具有在10nm至50,000nm之间的厚度e3。
图5是通过实施如上所述方法而涂覆的γ-TiAl基材201的照片。基材201涂覆有氧化铝层203并且在其表面具有包含钛、铝和氧的层204。
出于比较的目的，图6是通过非本发明的方法涂覆有氧化铝层303的γ-TiAl基材301的照片，该方法不包括铝层的初始沉积。基材在其表面还具有包含钛、铝和氧的层304。
可以观察到，上述方法的实施显著减少了在金属基材的涂覆过程中存在于基材表面的贫铝区域(图5中的202和图6中的302)。
在图5和图6所示的示例中，观察到的效果是，当氧化铝层通过本发明方法制备时，在涂覆的表面基材表面附近的贫铝区域为2μm厚(图5的区域202)，而当氧化铝层由非本发明方法制备时则为4μm(图6的区域302)。
在本发明中，除非另有明确说明，否则表述“包括在……和……之间”应理解为包括上限值和下限值。

Claims (13)

1.一种在包含铝的金属合金基材(11)的表面上形成氧化铝层(14)的方法，所述方法至少包括：
-在金属基材的表面上沉积第一铝层(12)，
-通过气相沉积在第一层上沉积第二层(13)，所述第二层包含铝、卤素和氧，以及
-在氧化气氛下对涂有第一层和第二层的基材进行热处理，以在金属基材的表面形成氧化铝层。
2.如权利要求1所述的方法，其中，第一铝层(12)的厚度e1在20nm至1000nm之间。
3.如权利要求1或2中任一项所述的方法，其中，所述卤素是氟。
4.如权利要求1至3中任一项所述的方法，其中，通过选自物理气相沉积、化学气相沉积、等离子体增强化学气相沉积和表面硬化的方法沉积第二层。
5.如权利要求1至4中任一项所述的方法，其中，所述第二层(13)的厚度大于或等于10μm。
6.如权利要求1至5中任一项所述的方法，其中，所述第二层(13)由包含氧、卤素气体和铝的气相沉积。
7.如权利要求6所述的方法，其中，通过在包含氧和卤素气体的气氛中对包含铝的靶(105)进行溅射来沉积第二层(13)。
8.如权利要求1至7中任一项所述的方法，其中，所述热处理在高于或等于800℃的温度下进行。
9.如权利要求1至8中任一项所述的方法，其中，所述金属基材(11)是铝化钛基合金。
10.如权利要求1至9中任一项所述的方法，其中，所述金属基材(11)是涡轮机部件。
11.一种经过涂覆的金属基材，其包含：
-包含铝的金属合金基材(11)，
-在金属基材表面上的第一铝层(12)，和
-包含铝、卤素和氧的第二层(13)，所述第二层涂覆于第一层。
12.如权利要求11所述的金属基材，其中，第一层(12)的厚度e1在20nm至1000nm之间。
13.如权利要求11或12中任一项所述的金属基材，其中，第二层(13)包含式AlOnFm的化合物，其中n和m各自严格地为正数。
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