Preparation, Microstructure and Mechanical Properties of Mo Layer and CoCrFeNiMn High Entropy Alloy Hard Coating Layer
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摘要: 为解决Invar合金在实际应用中硬度低、使用寿命有限的问题，采用双辉等离子表面合金化技术(double glow plasma surface alloying，DGPSA)在Invar合金表面制备了Mo及CoCrFeNiMn硬质涂层，使用X射线衍射、扫描电子显微镜和X射线能谱仪研究了2种涂层的相结构、微观结构及元素分布。采用纳米压痕法研究了加载应变率对2种硬质涂层表面硬度、弹性模量和蠕变性能的影响。结果显示：制备的Mo涂层厚度约为8.3 μm，涂层内部致密均匀，涂层具有体心立方结构；制备的CoCrFeNiMn涂层厚度约为10 μm，涂层内部存在少量孔隙，涂层具有面心立方结构。纳米压痕实验测得Mo涂层和CoCrFeNiMn涂层的硬度分别为15.49和8.18 GPa，弹性模量分别为278.70和227.12 GPa，2种硬质涂层均显著提高了Invar合金的表面硬度和弹性模量，且2种涂层均具有足够的韧性。2种涂层的硬度均随应变率的增大而增大，展现出明显的应变率效应，弹性模量基本保持稳定。同时，2种涂层的蠕变行为会受到加载应变率的影响，纳米压痕蠕变行为主要表现为位错运动，Mo涂层的改性效果优于CoCrFeNiMn涂层。
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关键词:
- 双辉等离子表面合金化技术 /
- 纳米压痕 /
- 应变率效应 /
- 蠕变性能
Abstract: To address the issue of low hardness and limited service life of the Invar alloy in practical applications, this study employs double-glow plasma surface alloying (DGPSA) technique to fabricate Mo and CoCrFeNiMn hard coating layers on the surface of the Invar alloy. The phase structure, microstructure, and element distribution of the two coating layers were investigated using X-ray diffraction (XRD), scanning electron microscope (SEM), and energy dispersive spectroscopy (EDS). The effects of loading strain rate on surface hardness, elastic modulus, and creep behavior of the two hard coating layers were systematically studied via nanoindentation. The thickness of the Mo coating layer is approximately 8.3 μm, with a dense and uniform internal structure and a body-centered cubic (BCC) structure. The thickness of the CoCrFeNiMn coating layer is approximately 10 μm, with some internal porosity and presents a face-centered cubic (FCC) structure. The nanoindentation tests show that the hardness of the Mo and CoCrFeNiMn coating layers is 15.49 and 8.18 GPa, respectively, while their elastic modulus are 278.70 and 227.12 GPa. The two hard coating layers significantly enhance the surface hardness and elastic modulus of the Invar alloy, and exhibit sufficient toughness. Hardness of the two coating layers increases with increasing strain rate, showing a pronounced strain rate sensitivity, while the elastic modulus remains relatively stable. Additionally, the creep behavior of the two coatings layers is influenced by the applied strain rate, with nanoindentation creep primarily governed by dislocation motion. The modification effect of the Mo coating layer is superior to that of the CoCrFeNiMn coating layer. -
图 1 CoCrFeNiMn涂层表面的SEM图像和EDS元素分布
Figure 1. SEM images and EDS element distribution of CoCrFeNiMn coating surface
图 2 CoCrFeNiMn和Mo涂层的XRD谱
Figure 2. XRD patterns of the CoCrFeNiMn layer and Mo coating layer
图 3 Mo涂层表面SEM图像和EDS元素分布
Figure 3. SEM images and EDS element distribution of the Mo coating surface
图 4 CoCrFeNiMn涂层的截面形态和EDS线扫图谱
Figure 4. Section morphology of the CoCrFeNiMn coating layer and EDS line scan map
图 5 Mo涂层的截面形态和相应的EDS线扫图谱
Figure 5. Section morphology of the Mo coating layer and corresponding EDS line scan map
图 6 不同应变率下2种涂层和Invar合金的载荷-位移曲线
Figure 6. Load-displacement curves of the two coating layers and Invar alloy at different strain rates
图 7 不同应变率下2种涂层和Invar合金的硬度-位移曲线
Figure 7. Hardness-displacement curves of the two coating layers and Invar alloy at different strain rates
图 8 不同应变率下2种涂层和Invar合金的弹性模量-位移曲线
Figure 8. Elastic modulus-displacement curves of the two coating layers and Invar alloy at different strain rates
图 9 2种涂层的硬度和弹性模量随应变率的变化
Figure 9. Variations of hardness and elastic modulus of the two coating layers with strain rates
图 10 不同应变率下2种涂层的蠕变位移和蠕变应变率随时间变化曲线
Figure 10. Creep displacement and creep strain rate versus time curves of the two coating layers at different strain rates
图 11 不同应变率下2种涂层的硬度与蠕变应变率的双对数曲线
Figure 11. Logarithmic curves of hardness and creep strain rate of the two coatings at different strain rates
表 1 Mo/CoCrCFeNiMn涂层的合金化工艺参数
Table 1. Process parameters of the Mo/CoCrFeNiMn coating layer
Distance between the source
and sample/mmVoltage of the
source/VVoltage of the
cathode/VWorking
pressure/PaHolding
time/hHolding
temperature/℃14–16 −920–−790 −620–−490 30 3 900 
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表 2 不同应变率下CoCrFeNiMn涂层的总功、弹性功、塑性功和塑性指数
Table 2. Total work, elastic work, plastic work and plastic index of the CoCrFeNiMn coating layer at different strain rates
$\dot \varepsilon $/s−1 Wtot/(10−9 J) We/(10−9 J) Wp/(10−9 J) i 0.01 33.52 10.71 22.81 0.68 0.05 44.38 15.62 28.76 0.65 0.10 46.71 18.96 27.75 0.59 0.20 61.29 24.36 36.93 0.60
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表 3 不同应变率下Mo涂层的总功、弹性功、塑性功和塑性指数
Table 3. Total work, elastic work, plastic work and plastic index of the Mo coating layer at different strain rates
$\dot \varepsilon$/s−1 Wtot/(10−9 J) We/(10−9 J) Wp/(10−9 J) i 0.01 75.81 23.51 52.30 0.69 0.05 78.47 23.62 54.85 0.70 0.10 87.36 31.32 56.04 0.64 0.20 97.32 34.82 62.50 0.64
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表 4 不同应变率下 Mo涂层的蠕变位移拟合结果
Table 4. Creep displacement fitting results of the Mo coating layer at different strain rates
$\dot \varepsilon $/s−1 A b k R2 0.01 3.53710 0.29675 0.01199 0.99583 0.05 10.99365 0.16660 0.01215 0.99604 0.10 10.11826 0.21823 − 0.00258 0.99658 0.20 21.23843 0.12993 0.01640 0.99750
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表 5 不同应变率下CoCrFeNiMn 涂层的蠕变位移拟合结果
Table 5. Creep displacement fitting results of the CoCrFeNiMn coating layer at different strain rates
$\dot \varepsilon $/s−1 A b k R2 0.01 3.36007 0.32704 − 0.01699 0.98791 0.05 3.57775 0.29970 0.00631 0.99523 0.10 11.15359 0.13845 0.00858 0.99193 0.20 10.30795 0.20805 0.00379 0.99692
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