CN109136849B - 一种Pt改性的梯度Al涂层及其制备方法 - Google Patents

一种Pt改性的梯度Al涂层及其制备方法 Download PDF

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CN109136849B
CN109136849B CN201810955190.0A CN201810955190A CN109136849B CN 109136849 B CN109136849 B CN 109136849B CN 201810955190 A CN201810955190 A CN 201810955190A CN 109136849 B CN109136849 B CN 109136849B
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孙超
孙健
刘书彬
李伟
姜肃猛
宫俊
何平
刘山川
褚天义
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Abstract

本发明公开了一种Pt改性的梯度Al涂层及其制备方法，属于高温防护涂层技术领域。首先采用电弧离子镀，在高温合金基体上镀一层MCrAlY底层；然后采用电镀的方法在MCrAlY底层上镀一层纯Pt层，并且在真空条件下进行退火；最后采用电弧离子镀在表面镀一层纯Al顶层并进行相应的退火处理，获得Pt改性梯度Al涂层。该涂层外层富Al内层富Cr，外层为β‑(Ni,Pt)Al和PtAl2相。本发明的优点：可以显著增加MCrAlY底层中的Al含量，提高其抗高温氧化性能；涂层的中Pt元素含量和涂层厚度可控。

Description

一种Pt改性的梯度Al涂层及其制备方法
技术领域
本发明涉及高温防护涂层技术领域，具体涉及一种Pt改性的梯度Al涂层及其制备方法。
技术背景
MCrAlY涂层广泛的应用在燃气轮机叶片和其他热端的部件作为高温防护涂层，MCrAlY涂层中的Al含量一般在8～16wt.％。在高温服役环境中，涂层表面形成致密的Al2O3膜，起到保护作用，但是Al元素被大量的消耗，所以MCrAlY涂层的抗氧化性能和服役寿命很大程度上取决于涂层中的Al含量。但是直接增加MCrAlY涂层中的Al含量会导致涂层的熔点降低，脆性增加。如果采用复合涂层或者梯度涂层设计可以很好的解决这一问题，同时可以提高MCrAlY涂层中的Al含量提高其抗高温氧化性能。相关应用文献如：①中国发明专利，一种MCrAlY加复合梯度涂层及制备工艺，申请号200710011431.8；②中国发明专利，一种共沉积梯度MCrAlY涂层及制备工艺，申请号200710011432.2；③中国发明专利，一种MCrAlY+AlSiY复合涂层及制备工艺，申请号200810228097.6等。
Pt是一种贵金属，化学性质极其稳定。Pt的添加提高了铝化物涂层中氧化膜与涂层的结合力，抑制了氧化膜的剥落。氧化膜的结合力对高温防护涂层的性能及寿命至关重要，良好的结合力可抑制氧化膜的剥落，减缓涂层中Al元素的消耗，从而延长了涂层寿命。因此考虑到Pt改性铝化物涂层和梯度MCrAlY涂层的优点，本发明提供了一种制备Pt改性的梯度Al涂层及其制备方法。
发明内容
本发明的目的在于提供一种Pt改性的梯度Al涂层及其制备方法，利用电弧离子镀和电镀相结合制备了Pt改性的梯度Al涂层，该涂层在不导致涂层的熔点降低、脆性增加的前提下，增加MCrAlY涂层中的Al含量，提高MCrAlY涂层的抗高温氧化和热腐蚀性能。
为实现上述目的，本发明所采用的技术方案如下：
一种Pt改性的梯度Al涂层的制备方法，该方法包括以下步骤：
(1)MCrAlY底层的制备：采用电弧离子镀在高温合金基体上制备MCrAlY底层；
(2)纯Pt层的制备：采用电镀方法在MCrAlY底层上制备一层纯Pt层；
(3)一次真空退火处理：电镀纯Pt层后在真空退火炉中进行一次退火处理，处理过程为：首先升温到500～700℃保温1～3h，以除去纯Pt层中残留的H2；然后升温到900～1000℃保温3～5h，以使纯Pt层和MCrAlY底层发生互扩散，保温结束后随炉冷却到室温；
(4)纯Al顶层的制备：采用电弧离子镀在纯Pt层上镀一层纯Al顶层；
(5)二次真空退火处理：升温到1000-1100℃保温1-5h，然后随炉冷却到室温；经二次真空退火处理后，在高温合金基体上获得Pt改性的梯度Al涂层。
上述步骤(1)中，高温合金基体在制备MCrAlY底层前，进行表面处理，表面处理过程为：对基体进行打磨和喷砂处理后，先在去离子水中超声15～30min，然后在丙酮中超声15～30min。
上述步骤(1)中，所述电弧离子镀过程为：首先将真空室的真空度抽到6.0×10-3～1.0×10-2Pa，通入高纯Ar气，压强升到5.0×10-2～3.0×10-1Pa；然后对基体进行溅射清洗，清洗工艺参数为：靶材和样品间的距离为200～300mm，脉冲偏压为-400～-800V，占空比为20～40％，清洗时间为5～8min；然后沉积MCrAlY底层，工艺参数为：靶材和样品间的距离为200～300mm，弧电压为20～25V，弧电流为60～100A，脉冲偏压为-100～-250V，占空比为20～40％，沉积时间为200～500min。
上述步骤(1)中，制备的MCrAlY底层的厚度为25～40μm。
上述步骤(2)中，采用电镀方法制备纯Pt层过程中，采用的镀液组成为：二亚硝基二胺合铂(以Pt当量计算)4～10g/L，其余为去离子水；镀液pH值为1-3；电镀时镀液温度为50～90℃，电流密度为2～8A/dm2，电镀时间为25～60min。镀Pt层的厚度为1～6μm。
上述步骤(3)中，经一次真空退火处理后，纯Pt层和MCrAlY底层发生互扩散，且分布均匀，Pt元素向MCrAlY底层扩散深度为10～18μm。
上述步骤(4)中，采用电弧离子镀制备纯Al顶层时，镀膜时间为60-180min，纯Al顶层厚度为10-30μm。
上述步骤(5)中，经二次退火处理，Pt层和纯Al顶层发生扩散。
上述步骤(3)和步骤(5)中，在一次和二次真空退火处理过程中，压强小于1.0×10-3Pa，升温速率小于8℃/min。
本发明具有以下优点：
1、采用电弧离子镀和电镀相结合，制备出外层富Al、内层富Cr的梯度涂层。通过调节Pt层、纯Al层的厚度及真空热处理工艺，可以控制涂层的化学成分和厚度。
2、与常规的MCrAlY高温防护涂层相比，在不降低涂层力学性能的条件下，提高了涂层内部的Al含量，使得涂层内的Al源能给表面氧化铝膜更长时间的补充，从而延缓涂层的退化，从而提高涂层的服役时间。
3、所制备的Pt改性梯度Al涂层具有优异的抗高温氧化性能和热腐蚀性能，能有效的保护基体合金，显著的提高发动机热端部件的使用寿命。
附图说明
图1为MCrAlY底层的截面形貌。
图2为电镀Pt后截面形貌。
图3为电镀Pt退火后截面形貌。
图4为镀完纯Al顶层后涂层的截面形貌。
图5为Pt改性梯度Al涂层的截面形貌。
图6为Pt改性梯度Al涂层的XRD图谱。
具体实施方式
以下结合附图和实施例详述本发明。
实施例1
本实施例是在镍基高温合金上制备Pt改性梯度Al涂层，所用的镍基单晶高温合金的成分为(wt.％)：Co 10.0％，Cr 8.0％，W 11.0％，Al 6.0％，Ti 1.0％，Mo 1.0％，Nb1.5％，C 0.05％，余量为Ni。涂层制备过程如下：
首先对基体进行打磨、喷砂，并且在去离子水和丙酮中先后超声30min。用酒精清洗后烘干待用。采用电弧离子镀沉积MCrAlY涂层时，预抽真空至7×10-3Pa，轰击和沉积时通入高纯Ar气，真空度为2×10-1Pa。对样品进行预溅射轰击清洗时，靶基距为240mm，脉冲偏压为-600V，占空比33％，清洗时间5min；沉积时，靶基距为240mm，弧电压为20V，弧电流为60～65A，脉冲偏压为-250V，占空比33％，沉积温度为300℃，沉积时间为400min，获得的涂层厚度约为30μm左右，图1为MCrAlY底层的截面形貌；
然后进行电镀Pt，对MCrAlY底层进行电化学除油、活化、预镀Ni处理，以提高底层和Pt层之间的结合力。电化学除油的具体工艺参数为：在5wt.％的NaOH水溶液中，样品作为阴极，阳极为纯Ni板，在8A/dm2的电流密度下除油60s。活化工艺参数为：37wt.％浓盐酸和去离子水按照体积比1:4混合，将样品放入其中活化30s后取出。预镀Ni过程中：镀液组成为：氯化镍200g/L，盐酸200ml/L，其余为去离子水；将样品作为阴极放入镀液中，在8A/dm2的电流密度下预镀Ni一分钟，阳极为纯镍板。用去离子水清洗样品后，将样品作为阴极放入镀Pt液中，具体的镀Pt工艺如下：温度80℃，电流密度3A/dm2，镀Pt液pH为2.0，铂钛网为阳极。镀Pt液组成为：二亚硝基二胺合铂(以Pt当量计算)4g/L，其余为去离子水。电镀时间为35min，Pt层厚度为2μm左右，图2为电镀Pt层后截面形貌；
电镀完成后，将样品进行扩散退火，以降低样品表面的Pt含量。退火的具体工艺为：升温速率为5℃/min，现在650℃除氢2.5h，然后在900℃扩散4h，最后随炉冷却，图3为电镀Pt退火后截面形貌；
采用电弧离子镀沉积纯Al顶层时，预抽真空至7×10-3Pa，轰击和沉积时通入高纯Ar气，真空度为2×10-1Pa。对样品进行预溅射轰击清洗时，靶基距为240mm，脉冲偏压为-600V，占空比33％，清洗时间5min；沉积时，靶基距为240mm，弧电压为20V，弧电流为60～65A，脉冲偏压为-250V，占空比33％，沉积温度为300℃，沉积时间为400min，获得的涂层厚度约为20μm左右，图4为镀完纯Al顶层后涂层的截面形貌；
沉积完Al顶层后，将样品进行扩散退火。退火的具体工艺为：升温速率5℃/min；在1050℃保温3.5h，然后随炉冷却到室温，喷砂去除表面扩散孔洞后得到Pt改性梯度Al涂层，图5为Pt改性梯度Al涂层的截面形貌；
本实施例中，采用XRD检测涂层的相组成。根据图6涂层的XRD图谱分析，涂层外层主要由β-(Ni,Pt)Al及PtAl2相组成。
以上所述仅为发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (8)

1.一种Pt改性的梯度Al涂层的制备方法，其特征在于：该方法包括以下步骤：
(1)MCrAlY底层的制备：采用电弧离子镀在高温合金基体上制备MCrAlY底层；所述电弧离子镀过程为：首先将真空室的真空度抽到6.0×10-3～1.0×10-2Pa，通入高纯Ar气，压强升到5.0×10-2～3.0×10-1Pa；然后对基体进行溅射清洗，清洗工艺参数为：靶材和样品间的距离为200～300mm，脉冲偏压为-400～-800V，占空比为20～40％，清洗时间为5～8min；然后沉积MCrAlY底层，工艺参数为：靶材和样品间的距离为200～300mm，弧电压为20～25V，弧电流为60～100A，脉冲偏压为-100～-250V，占空比为20～40％，沉积时间为200～500min；
(2)纯Pt层的制备：采用电镀方法在MCrAlY底层上制备一层纯Pt层；采用电镀方法制备纯Pt层过程中，采用的镀液组成为：二亚硝基二胺合铂(以Pt当量计算)4～10g/L，其余为去离子水；镀液pH值为1～3；电镀时镀液温度为50～90℃，电流密度为2～8A/dm2，电镀时间为25～60min；
(3)一次真空退火处理：电镀纯Pt层后在真空退火炉中进行一次退火处理，处理过程为：首先升温到500～700℃保温1～3h，以除去纯Pt层中残留的H2；然后升温到900～1000℃保温3～5h，以使纯Pt层和MCrAlY底层发生互扩散，保温结束后随炉冷却到室温；
(4)纯Al顶层的制备：采用电弧离子镀在纯Pt层上镀一层纯Al顶层；
(5)二次真空退火处理：升温到1000-1100℃保温1-5h，然后随炉冷却到室温；经二次真空退火处理后，在高温合金基体上获得Pt改性的梯度Al涂层。
2.根据权利要求1所述的Pt改性的梯度Al涂层的制备方法，其特征在于：步骤(1)中，高温合金基体在制备MCrAlY底层前，进行表面处理，表面处理过程为：对基体进行打磨和喷砂处理后，先在去离子水中超声15～30min，然后在丙酮中超声15～30min。
3.根据权利要求1所述的Pt改性的梯度Al涂层的制备方法，其特征在于：步骤(1)中，制备的MCrAlY底层的厚度为25～40μm。
4.根据权利要求1所述的Pt改性的梯度Al涂层的制备方法，其特征在于：步骤(2)中，镀Pt层的厚度为1～6μm。
5.根据权利要求1所述的Pt改性的梯度Al涂层的制备方法，其特征在于：步骤(3)中，经一次退火处理后，纯Pt层和MCrAlY底层发生互扩散，Pt元素向MCrAlY底层扩散深度为10～18μm。
6.根据权利要求1所述的Pt改性的梯度Al涂层的制备方法，其特征在于：步骤(4)中，采用电弧离子镀制备的纯Al顶层，其厚度为10-30μm。
7.根据权利要求1所述的Pt改性的梯度Al涂层的制备方法，其特征在于：步骤(3)和步骤(5)中，在一次和二次真空退火处理过程中，压强小于1.0×10-3Pa，升温速率小于8℃/min。
8.利用权利要求1所述方法制备的Pt改性的梯度Al涂层。
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