CN110079775B - 一种钼合金表面MoSi2涂层的制备方法 - Google Patents
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- 239000011248 coating agent Substances 0.000 title claims abstract description 66
- 229910001182 Mo alloy Inorganic materials 0.000 title claims abstract description 47
- 239000000956 alloy Substances 0.000 claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 41
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 37
- 238000004544 sputter deposition Methods 0.000 claims abstract description 26
- 229910016006 MoSi Inorganic materials 0.000 claims abstract description 21
- 229910020968 MoSi2 Inorganic materials 0.000 claims abstract description 20
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 19
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011733 molybdenum Substances 0.000 claims abstract description 16
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- 238000000034 method Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
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- 239000001301 oxygen Substances 0.000 claims description 6
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- 239000002245 particle Substances 0.000 claims description 2
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- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 abstract description 12
- 239000011159 matrix material Substances 0.000 abstract description 8
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- 238000005516 engineering process Methods 0.000 description 3
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- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
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- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 238000004372 laser cladding Methods 0.000 description 1
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- 230000008018 melting Effects 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
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Abstract
本发明涉及一种钼合金表面MoSi2涂层的制备方法，具体的为：(1)对钼合金表面进行抛光、清洗、烘干；(2)在钼合金表面溅射10‑20μm厚的ZrB2薄层；(3)按以下重量百分比配制合金粉末：Mo 52‑63％、Nb 3.0‑8.0％、Ti 2.0‑3.5％、W 3.0‑6.0％，余量为Si，将合金粉末进行球磨；(4)将合金粉末预置在ZrB2薄层上；(5)用激光器对预置有合金粉末的钼合金进行激光扫描，制成表面MoSi2涂层。本发明在钼合金和MoSi2涂层之间溅射一层ZrB2薄层，ZrB2薄层能够阻碍硅化物涂层主体中的Si元素向难熔金属基体内部扩散，可以有效提高MoSi2涂层的服役寿命。
Description
技术领域
本发明属于难熔金属表面工程技术领域，具体涉及一种钼合金表面MoSi2涂层的制备方法。
背景技术
钼基合金，熔点高，热膨胀系数小，弹性模量高，且具有良好的机械稳定性及优异的高温抗蠕变性能，在航天工程领域有着广泛的应用和发展前景。但钼的高温抗氧化性能较差，在725℃时即出现氧化物挥发，发生“灾害性”氧化，影响了在高温条件下的长期有效使用。
目前改善钼高温氧化性能的主要方法是在其表面制备硅化物涂层实现防护。在硅化物涂层中，MoSi2的高温抗氧化能力非常优异，高温下发生氧化时在表面形成致密的非晶态SiO2，可阻挡氧向内部扩散，而且非晶态SiO2具有流动性，能够弥补氧化进程中出现的微裂纹从而使涂层有自愈能力，可有效保护钼基体不被氧化。
在难熔金属/硅化物涂层体系的高温服役过程中，硅化物涂层主体中的Si元素将向难熔金属基体内部扩散，在难熔金属/硅化物涂层界面处形成新的过渡层，这一过程会加速涂层的组织退化和失效，因此，设计与构筑具有阻扩散作用的难熔金属硅化物涂层体系，阻碍涂层主体和基体元素之间的元素扩散至关重要。
发明内容
本发明主要提供了一种钼合金表面MoSi2涂层的制备方法，在钼合金和MoSi2涂层之间溅射一层ZrB2薄层，通过随后的激光扫描工艺在这一薄层上制备MoSi2涂层，ZrB2薄层能够阻碍硅化物涂层主体中的Si元素向难熔金属基体内部扩散，可以有效提高MoSi2涂层的服役寿命。其技术方案如下：
一种钼合金表面MoSi2涂层的制备方法，包括以下步骤：
(1)对钼合金表面进行抛光、清洗、烘干；
(2)在钼合金表面溅射10-20μm厚的ZrB2薄层；
(3)按以下重量百分比配制合金粉末：Mo 52-63％、Nb 3.0-8.0％、 Ti 2.0-3.5％、W 3.0-6.0％，余量为Si，将合金粉末进行球磨；
(4)将合金粉末预置在ZrB2薄层上；
(5)用激光器对预置有合金粉末的钼合金进行激光扫描，制成表面MoSi2涂层。
优选的，步骤(2)中溅射的方法为磁控溅射，使用高纯氩气作为溅射气体，氩气气流量为25-35sccm，氩气溅射气压为0.15-0.35Pa。
优选的，步骤(3)中元素Mo、Nb、Ti、W和Si均以合金粉末的形式加入，各元素粉末纯度大于99.5％，颗粒直径小于4.5μm。
优选的，步骤(3)中球磨时间为18-24h，转速为300-450r/min。
优选的，步骤(4)中合金粉末预置在ZrB2薄层上的方法为，采用酒精或丙酮将合金粉末粘附在ZrB2薄层上，预置合金粉末厚度为 0.8-1.2mm，随后将其放置于140-160℃加热炉中，干燥30-40min。
优选的，步骤(5)中激光扫描的搭接率为40-60％，激光功率为 2.0-2.5kW，扫描速度为4-8mm/s。
为了抑制或降低难熔金属基体与硅化物涂层之间的元素扩散，合理设计与基体和硅化物均能实现良好界面匹配的阻扩散层是一种直接有效的解决方法。ZrB2与Mo基合金及MoSi2都有很好的界面相容性，不会发生明显的界面反应。ZrB2弹性模量及热膨胀系数均与Mo 合金及MoSi2较为接近，可以避免因弹性模量及热膨胀系数的差异导致硅化钼涂层在受到热疲劳或热冲击时发生剥落。而且，ZrB2的阻扩散能力很强，可以很好的阻止Mo合金及MoSi2之间元素的互扩散。
采用合适的工艺有利于提高ZrB2与涂层主体及基体之间的界面结合强度，在本专利中，我们采用磁控溅射的方法在钼合金和MoSi2涂层的界面处制备ZrB2薄层，精确的控制ZrB2薄层厚度，有效抑制钼合金和MoSi2涂层之间的元素扩散。在制备钼合金表面MoSi2涂层时，在钼合金上溅射ZrB2薄层、随后预置MoSi2粉末涂层，采用激光扫描加工工艺将钼合金、溅射ZrB2薄层、预置MoSi2粉末涂层结合起来，激光熔覆技术具有稀释度小、组织致密、涂层与基体结合好等特点，可以改善钼合金表面的耐磨、耐蚀、耐热、抗氧化等性能。而在钼合金和MoSi2粉末涂层之间溅射ZrB2薄层的工艺，能够阻碍硅化物涂层主体中的Si元素向钼基体内部扩散，可以有效提高MoSi2涂层的服役寿命，从而改善和提高钼合金表面MoSi2涂层的综合性能。
ZrB2薄层的阻扩散效应可通过涂层的氧化实验时的质量变化进行测定。MoSi2在高温下长时间氧化时会发生以下化学反应：
2Mo5Si3+21O2→6SiO2+10MoO3
该化学反应由于MoO3具有挥发性，会导致质量下降。在高温 1500℃静态热氧空气中氧化时，MoSi2会缓慢失重。
由于本发明在钼合金和MoSi2涂层之间溅射一层ZrB2薄层，该薄层可以有效阻止Si元素和氧原子向涂层主体的扩散，使得涂层的氧化速度减慢，可有效减少上述化学反应的发生，降低涂层氧化的质量变化。因此可以通过128h的1500℃高高温氧化实验后涂层的质量变化来判断涂层的阻扩散效应。
采用上述方案，本发明具有以下优点：
本发明首次在钼合金表面溅射ZrB2薄层，随后通过激光扫描将钼合金、溅射ZrB2薄层和MoSi2涂层结合在一起，能够阻碍硅化物涂层主体中的Si元素向钼基体内部扩散，可以有效提高MoSi2涂层的服役寿命，因而溅射ZrB2薄层是在钼合金表面制备MoSi2涂层的非常适合的工艺方法。本发明的钼合金表面MoSi2涂层采用较先进的制备工艺，生产成本不高，综合性能优良。
具体实施方式
以下实施例中的实验方法如无特殊规定，均为常规方法，所涉及的实验试剂及材料如无特殊规定均为常规生化试剂和材料。
实施例1
首先对钼合金进行表面抛光，用酒精进行超声波清洗，烘干，随后通过磁控溅射钼合金上溅射15μm厚度的ZrB2薄层，使用高纯氩气作为溅射气体，氩气气流量为25sccm，氩气溅射气压为0.25Pa。将质量百分比为Mo 63％、Nb 3.0％、Ti2.0％、W 3.0％，余量为Si 的合金粉末进行长时间球磨，球磨时间为18h，转速为300r/min。此后采用丙酮将合金粉末粘附在溅射Si薄层的钼合金表面，预置合金粉末厚度为1.0mm，随后将其放置于140℃加热炉中，干燥30min。采用激光器对溅射ZrB2薄层的钼合金进行激光扫描，激光扫描的搭接率为40％，激光功率2.2kW，扫描速度8mm/s，制成表面MoSi2涂层。
经检测涂层在128h的1500℃静态热氧空气中能有效服役，质量损失为0.78％。
实施例2
首先对钼合金进行表面抛光，用酒精进行超声波清洗，烘干，随后通过磁控溅射钼合金上溅射15μm厚度的ZrB2薄层，使用高纯氩气作为溅射气体，氩气气流量为25sccm，氩气溅射气压为0.25Pa。将质量百分比为Mo 58％、Nb 5.5％、Ti 2.5％、W 4.5％，余量为Si 的合金粉末进行长时间球磨，球磨时间为21h，转速为350r/min。此后采用丙酮将合金粉末粘附在溅射ZrB2薄层的钼合金表面，预置合金粉末厚度为1.2mm，随后将其放置于150℃加热炉中，干燥30 min。采用激光器对溅射ZrB2薄层的钼合金进行激光扫描，激光扫描的搭接率为40％，激光功率2.5kW，扫描速度6mm/s，制成表面 MoSi2涂层。
经检测涂层在128h的1500℃静态热氧空气中能有效服役，质量损失为0.72％。
实施例3
首先对钼合金进行表面抛光，用酒精进行超声波清洗，烘干，随后通过磁控溅射钼合金上溅射20μm厚度的ZrB2薄层，使用高纯氩气作为溅射气体，氩气气流量为25sccm，氩气溅射气压为0.25Pa。将质量百分比为Mo 52％、Nb 8.0％、Ti 3.5％、W 6.0％，余量为Si 的合金粉末进行长时间球磨，球磨时间为24h，转速为400r/min。此后采用丙酮将合金粉末粘附在溅射ZrB2薄层的钼合金表面，预置合金粉末厚度为0.8mm，随后将其放置于160℃加热炉中，干燥40 min。采用激光器对溅射Si薄层的钼合金进行激光扫描，激光扫描的搭接率为40％，激光功率2.0kW，扫描速度8mm/s，制成表面MoSi2涂层。
经检测涂层在128h的1500℃静态热氧空气中能有效服役，质量损失为0.65％。
对比例1
首先对钼合金进行表面抛光，用酒精进行超声波清洗，烘干。将质量百分比为Mo63％、Nb 3.0％、Ti 2.0％、W 3.0％，余量为Si 的合金粉末进行长时间球磨，球磨时间为18h，转速为300r/min。此后采用丙酮将合金粉末粘附在钼合金表面，预置合金粉末厚度为1.0 mm，随后将其放置于140℃加热炉中，干燥30min。采用激光器对钼合金进行扫描，激光扫描的搭接率为40％，激光功率2.2kW，扫描速度8mm/s，制成表面MoSi2涂层。
经检测涂层在128h氧化后，质量损失为1.32％。
经实施例1与对比例1比较可知，在相同激光工艺参数下，实施例1涂层质量损失明显减少。
对本领域的技术人员来说，可根据以上描述的技术方案以及构思，做出其它各种相应的改变以及形变，而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。
Claims (6)
1.一种钼合金表面MoSi2涂层的制备方法，其特征在于：包括以下步骤：
(1)对钼合金表面进行抛光、清洗、烘干；
(2)在钼合金表面溅射10-20μm厚的ZrB2薄层；
(3)按以下重量百分比配制合金粉末：Mo 52-63％、Nb 3.0-8.0％、Ti 2.0-3.5％、W3.0-6.0％，余量为Si，将合金粉末进行球磨；
(4)将合金粉末预置在ZrB2薄层上；
(5)用激光器对预置有合金粉末的钼合金进行激光扫描，制成表面MoSi2涂层；
所述涂层能够在128h的1500℃静态热氧空气中有效服役。
2.根据权利要求1所述的钼合金表面MoSi2涂层的制备方法，其特征在于：步骤(2)中溅射的方法为磁控溅射，使用高纯氩气作为溅射气体，氩气气流量为25-35sccm，氩气溅射气压为0.15-0.35Pa。
3.根据权利要求1所述的钼合金表面MoSi2涂层的制备方法，其特征在于：步骤(3)中元素Mo、Nb、Ti、W和Si均以合金粉末的形式加入，各元素粉末纯度大于99.5％，颗粒直径小于4.5μm。
4.根据权利要求1所述的钼合金表面MoSi2涂层的制备方法，其特征在于：步骤(3)中球磨时间为18-24h，转速为300-450r/min。
5.根据权利要求1所述的钼合金表面MoSi2涂层的制备方法，其特征在于：步骤(4)中合金粉末预置在ZrB2薄层上的方法为，采用酒精或丙酮将合金粉末粘附在ZrB2薄层上，预置合金粉末厚度为0.8-1.2mm，随后将其放置于140-160℃加热炉中，干燥30-40min。
6.根据权利要求1所述的钼合金表面MoSi2涂层的制备方法，其特征在于：步骤(5)中激光扫描的搭接率为40-60％，激光功率为2.0-2.5kW，扫描速度为4-8mm/s。
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