镁合金表面磁控溅射沉积Cr基涂层的结构与特性研究
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摘要
Mg合金是未来最有潜力的结构材料之一,但表面质软和易腐蚀是需要解决的重要问题。虽然当前应用在Mg合金上的表面处理技术改善了Mg合金表面的性能,但所制备的涂层在结合性能、摩擦磨损以及机械性能均不能满足Mg合金在关键零部件领域的应用。磁控溅射是目前主流的PVD表面处理技术之一,制备的涂层具有结合性能强和致密度高的优点;所需的沉积温度低,可以满足Mg合金低工艺温度的要求。因此,磁控溅射技术沉积硬质涂层为改善Mg合金表面的摩擦磨损提供了一种思路。
在目前的研究工作中,采用平面磁控溅射技术在Mg合金上沉积CrNx涂层和CrNxOyCz涂层,并通过扫描电镜(SEM)、光电子能谱(XPS)以及X-射线衍射(XRD)等分析技术对涂层的结构特性进行了表征。采用非平衡闭合磁场磁控溅射离子镀技术沉积CrTiAlN涂层,通过透射电镜(TEM)、显微硬度仪以及摩擦磨损实验研究涂层在Mg上的界面结构、机械性能以及摩擦磨损性能。此外,还讨论了柱状晶的生长和表面轮廓的演化特征。主要研究结果如下:
①CrNx涂层的结构特性取决于沉积的工艺,包括衬底温度、N2浓度、靶电流密度以及衬底偏压。沉积速度是电流密度的二次增长函数关系,而增加的N2含量导致沉积速度呈指数的衰减。在Mg合金上的CrNx涂层随着N2浓度的增加则趋向于形成更为开放的边界。
②CrN涂层的沉积涉及到Cr桥接层、CrNx过渡层以及化学比的CrN层。Cr膜在镁合金上的柱状生长起源于网状膜,CrN涂层的柱状生长机制包括遮蔽和吞并。面内平均直径和粒度的方差σ2均与厚度呈线性关系,表面的粗糙度值与厚度呈现指数的关系。
③衬底表面轮廓在涂层表面的演化取决于涂层的厚度,表面轮廓随着涂层的增厚趋于平滑。由于相内粗化,表面粗糙度随着涂层的增厚而增加,同时偏置功率的增加也会导致表面轮廓的偏差减小。CrNx涂层的表面粗糙度与N原子浓度呈线性关系,与厚度呈指数关系。
④CrNxOyCz涂层为柱状生长,涂层中含有CrN、Cr2N、Cr3C2、Cr2O3、CrO2以及CrNxOy相;污染或氧化的O和C原子浓度在表面的深度分布服从衰减的一阶指数函数,涂层中的Cr3C2和Cr2N属于非稳定相。涂层的摩擦磨损特性比CrNx涂层的要差。
⑤AZ31-Mg合金的标准磨损率SWR达到1055×10-15m3·N-1·m-1,而在Mg合金上的CrTiAlN涂层的SWR只有2.4×10-15m3·N-1·m-1。偏压在-50V时CrTiAlN涂层的结合力达到10N。
⑥当在中N2水平和衬底偏压为-55V时,CrTiAlN涂层和摩擦副WC-Co6%球之间的磨损最小,摩擦系数能够稳定在0.2-0.3。CrTiAlN/MoS2涂层的摩擦磨损性能比CrTiAlN涂层明显改善,滑动摩擦循环次数Nc达到70000次,摩擦系数能够稳定在0.2-0.35之间。
It will be one of the prevalent structure materials in future for Mg alloy, which need to be treated due to soft surface and lower ability of corrosion resistance. Although the surface treatment technologies applied in Mg alloy have improved surface performance, adhesion force, frictional wear and mechanical property can not satisfy demand which Mg alloy is applied in key parts area. At present magnetron sputtering is one of the mainstream PVD (physical phase deposition) technologies, and the coating deposited demonstrated high adhesion force and density at lower deposition temperature. So, it proposed a method that the hard coatings were deposited by magnetron sputtering.
In present research, the CrNx and CrNxOyCz coatings on Mg alloy were deposited by planner magnetron sputtering and the structure property of coatings were characterized by scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD), respectively. The CrTiAlN coatings were deposited by closed field unbalanced magnetron sputtering ion plating (CFUBMS), and the structure, frictional wear and mechanical property were characterized by transmission electron microscope (TEM), frictional wear tester (ST3001) and microhardness tester, respectively. Moreover, the growth of columnar crystal and evolution of surface profile were discussed, the main results are as follows:
①Structure property of CrNx coatings depends on the technological parameters which include subastrate temperature, N2 content, current density of target and bias voltage of substrate. Deposition rate shows the quadratic increasing function of current density, while it demonstrates exponentially decay with increasing N2 content. The CrNx coatings on Mg alloy tend to form columnar crystal with open boundary with increasing in N2 content.
②Deposition of CrNx coatings is related to bridged Cr layer, transition CrNx layer and atomic CrN layer. The columnar growth of Cr film on Mg alloy originates from meshy growth. Growth of CrN coating on Mg alloy includes shadow and merger growth. The in-plane average diameter and variance of grain size (σ2) indicate linear growth with thickness increasing, and surface roughness presents exponential growth.
③Surface profile of coating which was affected by substrate surface depends on coating thickness, and tends to smooth with coating thickening if the roughness of in-phase is omitted. Surface roughness increases with film thickness thickening for in-phase roughness, and the increased bias power will result in decrease of surface roughness. It shows linear function between surface roughness of CrNx coatings and N atomic concentration, and exponential relationship between one and thickness.
④The CrNxOyCz coatings deposited in reactive atmosphere reveals columnar growth, several different species occur, including CrN, Cr2N, Cr3C2, Cr2O3, CrO2 and CrNxOy. The profile concentration Oxygen and Carbon atoms obey first order exponential decay function, and Cr3C2 and Cr2N belongs to unstable phase. The frictional wear property of CrNxOyCz coating is worse than that of CrNx coatings.
⑤The special wear rate (SWR) of AZ31 arrives at 1055×10-15m3·N-1·m-1, while that of CrTiAlN coatings on Mg alloy is 2.4×10-15m3·N-1·m-1. The adhesion force of CrTiAlN coatings at bias voltage (Vb) -50V reaches to 10N.
⑥The SWR of CrTiAlN coatings and WC-Co6% ball are the smallest at Vb=-55V and medium N2, and friction coefficient can stabilize at 0.2-0.3. Frictional wear property of CrTiAlN/MoS2 coating outperforms CrTiAlN coating, cycle index of sliding friction reaches to 70000, and friction coefficient can stabilize at 0.2-0.35.
在目前的研究工作中,采用平面磁控溅射技术在Mg合金上沉积CrNx涂层和CrNxOyCz涂层,并通过扫描电镜(SEM)、光电子能谱(XPS)以及X-射线衍射(XRD)等分析技术对涂层的结构特性进行了表征。采用非平衡闭合磁场磁控溅射离子镀技术沉积CrTiAlN涂层,通过透射电镜(TEM)、显微硬度仪以及摩擦磨损实验研究涂层在Mg上的界面结构、机械性能以及摩擦磨损性能。此外,还讨论了柱状晶的生长和表面轮廓的演化特征。主要研究结果如下:
①CrNx涂层的结构特性取决于沉积的工艺,包括衬底温度、N2浓度、靶电流密度以及衬底偏压。沉积速度是电流密度的二次增长函数关系,而增加的N2含量导致沉积速度呈指数的衰减。在Mg合金上的CrNx涂层随着N2浓度的增加则趋向于形成更为开放的边界。
②CrN涂层的沉积涉及到Cr桥接层、CrNx过渡层以及化学比的CrN层。Cr膜在镁合金上的柱状生长起源于网状膜,CrN涂层的柱状生长机制包括遮蔽和吞并。面内平均直径和粒度的方差σ2均与厚度呈线性关系,表面的粗糙度值与厚度呈现指数的关系。
③衬底表面轮廓在涂层表面的演化取决于涂层的厚度,表面轮廓随着涂层的增厚趋于平滑。由于相内粗化,表面粗糙度随着涂层的增厚而增加,同时偏置功率的增加也会导致表面轮廓的偏差减小。CrNx涂层的表面粗糙度与N原子浓度呈线性关系,与厚度呈指数关系。
④CrNxOyCz涂层为柱状生长,涂层中含有CrN、Cr2N、Cr3C2、Cr2O3、CrO2以及CrNxOy相;污染或氧化的O和C原子浓度在表面的深度分布服从衰减的一阶指数函数,涂层中的Cr3C2和Cr2N属于非稳定相。涂层的摩擦磨损特性比CrNx涂层的要差。
⑤AZ31-Mg合金的标准磨损率SWR达到1055×10-15m3·N-1·m-1,而在Mg合金上的CrTiAlN涂层的SWR只有2.4×10-15m3·N-1·m-1。偏压在-50V时CrTiAlN涂层的结合力达到10N。
⑥当在中N2水平和衬底偏压为-55V时,CrTiAlN涂层和摩擦副WC-Co6%球之间的磨损最小,摩擦系数能够稳定在0.2-0.3。CrTiAlN/MoS2涂层的摩擦磨损性能比CrTiAlN涂层明显改善,滑动摩擦循环次数Nc达到70000次,摩擦系数能够稳定在0.2-0.35之间。
It will be one of the prevalent structure materials in future for Mg alloy, which need to be treated due to soft surface and lower ability of corrosion resistance. Although the surface treatment technologies applied in Mg alloy have improved surface performance, adhesion force, frictional wear and mechanical property can not satisfy demand which Mg alloy is applied in key parts area. At present magnetron sputtering is one of the mainstream PVD (physical phase deposition) technologies, and the coating deposited demonstrated high adhesion force and density at lower deposition temperature. So, it proposed a method that the hard coatings were deposited by magnetron sputtering.
In present research, the CrNx and CrNxOyCz coatings on Mg alloy were deposited by planner magnetron sputtering and the structure property of coatings were characterized by scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD), respectively. The CrTiAlN coatings were deposited by closed field unbalanced magnetron sputtering ion plating (CFUBMS), and the structure, frictional wear and mechanical property were characterized by transmission electron microscope (TEM), frictional wear tester (ST3001) and microhardness tester, respectively. Moreover, the growth of columnar crystal and evolution of surface profile were discussed, the main results are as follows:
①Structure property of CrNx coatings depends on the technological parameters which include subastrate temperature, N2 content, current density of target and bias voltage of substrate. Deposition rate shows the quadratic increasing function of current density, while it demonstrates exponentially decay with increasing N2 content. The CrNx coatings on Mg alloy tend to form columnar crystal with open boundary with increasing in N2 content.
②Deposition of CrNx coatings is related to bridged Cr layer, transition CrNx layer and atomic CrN layer. The columnar growth of Cr film on Mg alloy originates from meshy growth. Growth of CrN coating on Mg alloy includes shadow and merger growth. The in-plane average diameter and variance of grain size (σ2) indicate linear growth with thickness increasing, and surface roughness presents exponential growth.
③Surface profile of coating which was affected by substrate surface depends on coating thickness, and tends to smooth with coating thickening if the roughness of in-phase is omitted. Surface roughness increases with film thickness thickening for in-phase roughness, and the increased bias power will result in decrease of surface roughness. It shows linear function between surface roughness of CrNx coatings and N atomic concentration, and exponential relationship between one and thickness.
④The CrNxOyCz coatings deposited in reactive atmosphere reveals columnar growth, several different species occur, including CrN, Cr2N, Cr3C2, Cr2O3, CrO2 and CrNxOy. The profile concentration Oxygen and Carbon atoms obey first order exponential decay function, and Cr3C2 and Cr2N belongs to unstable phase. The frictional wear property of CrNxOyCz coating is worse than that of CrNx coatings.
⑤The special wear rate (SWR) of AZ31 arrives at 1055×10-15m3·N-1·m-1, while that of CrTiAlN coatings on Mg alloy is 2.4×10-15m3·N-1·m-1. The adhesion force of CrTiAlN coatings at bias voltage (Vb) -50V reaches to 10N.
⑥The SWR of CrTiAlN coatings and WC-Co6% ball are the smallest at Vb=-55V and medium N2, and friction coefficient can stabilize at 0.2-0.3. Frictional wear property of CrTiAlN/MoS2 coating outperforms CrTiAlN coating, cycle index of sliding friction reaches to 70000, and friction coefficient can stabilize at 0.2-0.35.
引文
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