多弧离子镀Ti-Al-Zr-Cr-N系复合硬质膜的制备、微结构与性能
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摘要
在高速钢和硬质合金刀具表面沉积TiN等硬质膜,可提高刀具的硬度和耐磨性,从而提高刀具的切削性能和使用寿命。但随着数控加工机床的逐渐普及,高速切削已成为机械加工的主流,TiN薄膜刀具难以满足使用性能的要求。而另一方面,薄膜合金化、多层化和梯度化等复合形式可以实现提高硬质薄膜的综合性能和使用寿命。因此,本文旨在通过合金元素的添加和薄膜构成形式的变化来探索TiN基复合薄膜综合性能的改善。
采用多弧离子镀技术,使用两个Ti-Al-Zr合金靶和一个纯Cr靶,在W18Cr4V高速钢和WC-8%Co硬质合金两种基体上成功地沉积了四种Ti-Al-Zr-Cr-N系复合硬质膜,即(Ti,Al,Zr,Cr)N多元膜、(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N和CrN/(Ti,Al,Zr,Cr)N多元双层膜以及TiAlZrCr/(Ti,Al,Zr,Cr)N多元梯度膜。利用扫描电镜(SEM)、激光扫描共聚焦光学显微镜、电子能谱仪(EDS)和X射线衍射(XRD)对四种复合膜的成分、形貌、粗糙度和微观结构进行了测量和表征;利用显微硬度计和划痕仪测评了四种复合膜的硬度和膜/基结合力;利用摩擦磨损试验机研究了四种复合膜在常温(15℃)和高温(500℃)条件下的耐磨损特性,并采用SEM观察了磨痕的表面形貌;同时对四种复合膜进行了600℃、700℃、800℃和900℃短时(4h)高温氧化实验及700℃和800℃长时(100h)高温循环氧化实验,并利用SEM、EDS和XRD观察和分析了试样表面的氧化膜。
研究结果表明,获得的四种Ti-Al-Zr-Cr-N系复合硬质膜均具有B1-NaCl型的TiN面心立方结构;四种复合膜的成分除-50V偏压外,其它偏压下的变化均不明显;复合膜的表面都比较平整、致密,但仍然存在较多的大颗粒(微液滴)和微孔缺陷,同时增大偏压可以减少其表面的液滴污染现象,表面粗糙度有所改善;复合膜与基体之间无明显的缺陷,薄膜具有从基体到表面垂直生长的柱状晶组织;在不同的偏压下,四种复合膜的厚度大约为1～1.5μm,而且随着偏压的增大,其厚度有所减小。
高速钢和硬质合金基体上的(Ti,Al,Zr,Cr)N多元膜的(Al+Zr+Cr)/(Ti+Al+Zr+Cr)原子比值分别为0.44～0.52和0.41～0.43,当其分别趋于0.44和0.41时,薄膜的显微硬度分别达到最大值3300HV_(0.01)和3600HV_(0.01),膜/基结合力也分别达到最大值190N和200N。(Ti,Al,Zr,Cr)N多元膜的摩擦磨损机理均为以塑性变形为主要特征的粘着磨损,并伴有轻微的磨粒磨损。在常温和高温条件下磨损时,平均摩擦系数在0.3～0.5之间。薄膜的摩擦系数曲线和磨损表面形貌分析表明,随着沉积偏压的增加,其耐磨性有所提高,而且硬质合金基体略优于高速钢基体上薄膜的耐磨性。另外,在短时氧化条件下,高速钢和硬质合金基体上的(Ti,Al,Zr,Cr)N膜分别在800℃和700℃时具有良好的抗高温氧化性能,在XRD谱中观察到了金红石结构的TiO_2;在长时氧化条件下,高速钢和硬质合金基体上(Ti,Al,Zr,Cr)N膜的抗高温循环氧化温度分别为700℃和600℃。
(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N多元双层膜具有比(Ti,Al,Zr,Cr)N单层膜更高的硬度和更强的膜/基结合力。当高速钢和硬质合金基体上(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N膜的(Al+Zr+Cr)/(Ti+Al+Zr+Cr)原子比值分别达到0.44和0.40时,薄膜的显微硬度分别达到最大值3450HV_(0.01)和4000HV_(0.01),膜/基结合力也分别达到最大值190N和＞200N。同时,(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜具有比(Ti,Al,Zr,Cr)N单层膜更优的耐磨损性能,其在常温和高温下磨损时的平均摩擦系数在0.3～0.35之间。而且,氧化增重、氧化膜的表面形貌及其相结构的分析表明,(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜具有比(Ti,Al,Zr,Cr)N单层膜更为良好的抗高温氧化性能。
CrN/(Ti,Al,Zr,Cr)N多元双层膜具有比(Ti,Al,Zr,Cr)N单层膜更高、但略低于(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜的硬度,同时具有比(Ti,Al,Zr,Cr)N单层膜和(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜都强的膜/基结合力。当高速钢和硬质合金基体上CrN/(Ti,Al,Zr,Cr)N膜的(Al+Zr+Cr)/(Ti+Al+Zr+Cr)原子比值分别趋于0.45和0.40时,薄膜的显微硬度分别达到最大值3400HV_(0.01)和3900HV_(0.01),膜/基结合力也分别达到最大值190N和＞200N。同时,CrN/(Ti,Al,Zr,Cr)N双层膜具有比(Ti,Al,Zr,Cr)N单层膜更优、但略低于(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜的耐磨损性能,其在常温和高温下磨损时的平均摩擦系数分别在0.3～0.4和0.3～0.45之间。而且,CrN/(Ti,Al,Zr,Cr)N双层膜具有比(Ti,Al,Zr,Cr)N单层膜更为良好的抗高温氧化性能。在短时氧化条件下,硬质合金基体上CrN/(Ti,Al,Zr,Cr)N膜的抗高温氧化温度进一步提高到800℃。
TiAlZrCr/(Ti,Al,Zr,Cr)N多元梯度膜具有比(Ti,Al,Zr,Cr)N单层膜及(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N和CrN/(Ti,Al,Zr,Cr)N双层膜更高的硬度和更强的膜/基结合力。当高速钢和硬质合金基体上梯度膜的(Al+Zr+Cr)/(Ti+Al+Zr+Cr)原子比值分别达到0.45和0.39时,薄膜的显微硬度分别达到最大值3500HV_(0.01)和4000HV_(0.01),膜/基结合力也分别达到最大值200N和＞200N。同时,TiAlZrCr/(Ti,Al,Zr,Cr)N梯度膜具有比(Ti,Al,Zr,Cr)N单层膜及(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N和CrN/(Ti,Al,Zr,Cr)N双层膜更优的耐磨性,其在常温和高温下磨损时的平均摩擦系数分别在0.25～0.3和0.3～0.35之间。而且,在短时氧化条件下,高速钢和硬质合金两种基体上的TiAlZrCr/(Ti,Al,Zr,Cr)N梯度膜在800℃时均具有良好的抗高温氧化性能;在长时氧化条件下,高速钢和硬质合金两种基体上TiAlZrCr/(Ti,Al,Zr,Cr)N梯度膜的抗高温循环氧化温度均为700℃,与(Ti,Al,Zr,Cr)N单层膜及(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N和CrN/(Ti,Al,Zr,Cr)N双层膜相比,其抗高温氧化性能得到了明显的改善。
The TiN hard films deposited on the cutting tools of high speed steel and cemented carbide can enhance their hardness and wear resistance, which, in turn, improve the cutting performance and service life. However, high speed cutting has been the main trend in the mechanical processing field. The TiN hard films deposited cutting tools would not fulfill the function requirements of the numerical controlled processing machines, which gradually become more popular. On the other hand, the various composite techniques, namely film alloying, multilayer and gradient-layer, could improve the comprehensive quality and service life of the hard films. Therefore, the objective of this study is to achieve the better properties of TiN-based composite films by adding the different alloy elements and modifying the film structures.
The two Ti-Al-Zr targets and one pure Cr target were used to prepare four types of Ti-Al-Zr-Cr-N composite hard films, namely (Ti, Al, Zr, Cr) N multi-component films, (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films, CrN/(Ti, Al, Zr, Cr) N bilayered films and TiAlZrCr/(Ti, Al, Zr, Cr) N gradient films, on the substrates of high speed steel (W18Cr4V) and cemented carbide (WC-8%Co). The composition, morphology, roughness and microstructure of the films were analyzed by energy disperse X-ray spectroscopy (EDS), scanning electron microscopy (SEM), laser scanning Confocal optical microscopy and X-ray diffraction (XRD). Vickers indentation and scratch test were performed to measure the micro-hardness and the adhesive strength between the film and the substrate. Meanwhile, the wear resistance of the films was studied by abrasion tester at the room temperature (15℃) and elevated temperature (500℃), and the worn surface morphologies were studied by SEM. Furthermore, short-term isothermal (at 600℃, 700℃, 800℃and 900℃for 4h) and long-term cyclic (at 700℃ and 800℃for 100h) high temperature oxidation behaviors of the films were studied, and the oxide scales formed on the film specimens were characterized by SEM, EDS and XRD.
It was showed that the obtained Ti-Al-Zr-Cr-N composite hard films were of the TiN (B1-NaCl) type face-centered cubic structure. The compositions of the four composite films did not change too much at the other bias voltages except at -50V. The surface morphologies of the composite films were isotropy and dense; however, there were many macro-particles (or micro-drops) and pores. By increasing the bias voltage, the drop contamination on the films decreased significantly, and then the surface roughness of the films was also improved. The cross-section morphologies revealed the typical and dense columnar structure. No evident defects were observed at the interface between the composite films and the substrates. The thickness of the four composite films was about l~1.5|xm at the different bias voltages, and decreased with increasing the bias voltage.
In the (Ti, Al, Zr, Cr) N multi-component films, the atomic ratio of (Al+Zr+Cr)/ (Ti+Al+Zr+Cr) varied from 0.44 to 0.52 on the W18Cr4V substrates, whereas it varied from 0.41 to 0.43 on the WC-8%Co substrates. When the atomic ratio approached 0.44 and 0.41, the micro-hardness of the films was improved up to 3300HV_(0.01) and 3600HV_(0.01), respectively. The adhesive strength between the film and the substrate was also enhanced up to 190N and 200N, respectively. The wear behavior of the films was characterized by the adhesive wear that was caused by the plastic deformation feature and the slight abrasive wear. The average values of friction coefficient varied between 0.3 and 0.5 at the room temperature and elevated temperature in the (Ti, Al, Zr, Cr) N multi-component films. The friction coefficient curves and the worn surface morphologies showed that the wear resistance was improved as the bias voltage increased. The properties of the films on the WC-8%Co substrates were better than those on the W18Cr4V substrates. Moreover, under short-term isothermal condition, the (Ti, Al, Zr, Cr) N films presented the excellent high temperature oxidation resistance on both the W18Cr4V (up to 800℃) and WC-8%Co (up to 700℃) substrates, and an oxide scale of TiO_2 was observed by XRD. On the other hand, under long-term cyclic high temperature condition, the oxidation resistant temperature of the (Ti, Al, Zr, Cr) N films was about 700℃on the W18Cr4V substrates and 600℃on the WC-8%Co substrates.
The micro-hardness of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films and the adhesive strength between the bilayered film and the substrate were increased remarkably with the addition of (Ti, Al, Zr) N interlayer. When the atomic ratio of (Al+Zr+Cr)/(Ti+Al+Zr+Cr) reached 0.44 on the W18Cr4V substrates and 0.40 on the WC-8%Co substrates, the micro-hardness of the films was improved up to 3450HV_(0.01) and 4000HV_(0.01), respectively. The adhesive strength between the film and the substrate was also enhanced to 190N and above 200N, respectively. Meanwhile, the wear resistance of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films was superior to those of the (Ti, Al, Zr, Cr) N single-layered films. The average values of friction coefficient varied between 0.3 and 0.35 at the room temperature and elevated temperature in the bilayered films. Moreover, the high temperature oxidation resistance of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films was improved with the addition of (Ti, Al, Zr) N interlayer according to the analysis of mass gain, morphology and microstructure of the oxide scales.
In the CrN/(Ti, Al, Zr, Cr) N bilayered films, the micro-hardness values were higher than those of the (Ti, Al, Zr, Cr) N single-layered films, but lower than those of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films. The CrN/(Ti, Al, Zr, Cr) N bilayered films also presented the superior adhesive strength, as compared with (Ti, Al, Zr, Cr) N and (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N films. When the atomic ratio of (Al+Zr+Cr) /(Ti+Al+Zr+Cr) reached 0.45 on the W18Cr4V substrates and 0.40 on the WC-8%Co substrates, the micro-hardness of the films was improved up to 34OOHV_(0.01) and 3900HV_(0.01), respectively. The adhesive strength between the film and the substrate was also enhanced up to 190N and above 200N, respectively. Meanwhile, the wear resistance of the CrN/(Ti, Al, Zr, Cr) N bilayered films was superior to those of the (Ti, Al, Zr, Cr) N single-layered films, while not as good as those of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films. The average values of friction coefficient varied between 0.3 and 0.4 at the room temperature and varied between 0.3 and 0.45 at the elevated temperature in the CrN/(Ti, Al, Zr, Cr) N films. Moreover, the high temperature oxidation resistance of the CrN/(Ti, Al, Zr, Cr) N bilayered films was improved with the addition of CrN interlayer, in which the oxidation resistance temperature of the films on the WC-8%Co substrates was up to 800℃under the short-term isothermal oxidation condition.
The micro-hardness and adhesive strength of the TiAlZrCr/(Ti, Al, Zr, Cr) N gradient films were higher than those of the (Ti, Al, Zr, Cr) N, (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N and CrN/(Ti, Al, Zr, Cr) N films. When the atomic ratio of (Al+Zr+Cr)/(Ti +Al+Zr+Cr) approached 0.45 on the W18Cr4V substrates and 0.39 on the WC-8%Co substrates, the micro-hardness of the gradient films was enhanced up to 3500HV_(0.01) and 4000HV_(0.01), respectively. The adhesive strength between the gradient film and the substrate was also enhanced up to 200N and above 200N, respectively. Meanwhile, the wear resistance of the TiAlZrCr/(Ti, Al, Zr, Cr) N gradient films was superior to those of the (Ti, Al, Zr, Cr) N, (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N and CrN/(Ti, Al, Zr, Cr) N films. The average values of friction coefficient varied between 0.25 and 0.3 at the room temperature and varied between 0.3 and 0.35 at the elevated temperature in the gradient films. Moreover, under short-term isothermal condition, the high temperature oxidation resistance of the films was excellent up to 800℃on both the W18Cr4V and WC-8%Co substrates. Under long-term cyclic high temperature condition, the oxidation resistance of the films was excellent at about 700℃on both the W18Cr4V and WC-8%Co substrates. Therefore, the high temperature oxidation resistance of the TiAlZrCr/(Ti, Al, Zr, Cr) N gradient films was obviously improved and better than those of (Ti, Al, Zr, Cr) N, (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N and CrN/(Ti, Al, Zr, Cr) N films.
采用多弧离子镀技术,使用两个Ti-Al-Zr合金靶和一个纯Cr靶,在W18Cr4V高速钢和WC-8%Co硬质合金两种基体上成功地沉积了四种Ti-Al-Zr-Cr-N系复合硬质膜,即(Ti,Al,Zr,Cr)N多元膜、(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N和CrN/(Ti,Al,Zr,Cr)N多元双层膜以及TiAlZrCr/(Ti,Al,Zr,Cr)N多元梯度膜。利用扫描电镜(SEM)、激光扫描共聚焦光学显微镜、电子能谱仪(EDS)和X射线衍射(XRD)对四种复合膜的成分、形貌、粗糙度和微观结构进行了测量和表征;利用显微硬度计和划痕仪测评了四种复合膜的硬度和膜/基结合力;利用摩擦磨损试验机研究了四种复合膜在常温(15℃)和高温(500℃)条件下的耐磨损特性,并采用SEM观察了磨痕的表面形貌;同时对四种复合膜进行了600℃、700℃、800℃和900℃短时(4h)高温氧化实验及700℃和800℃长时(100h)高温循环氧化实验,并利用SEM、EDS和XRD观察和分析了试样表面的氧化膜。
研究结果表明,获得的四种Ti-Al-Zr-Cr-N系复合硬质膜均具有B1-NaCl型的TiN面心立方结构;四种复合膜的成分除-50V偏压外,其它偏压下的变化均不明显;复合膜的表面都比较平整、致密,但仍然存在较多的大颗粒(微液滴)和微孔缺陷,同时增大偏压可以减少其表面的液滴污染现象,表面粗糙度有所改善;复合膜与基体之间无明显的缺陷,薄膜具有从基体到表面垂直生长的柱状晶组织;在不同的偏压下,四种复合膜的厚度大约为1～1.5μm,而且随着偏压的增大,其厚度有所减小。
高速钢和硬质合金基体上的(Ti,Al,Zr,Cr)N多元膜的(Al+Zr+Cr)/(Ti+Al+Zr+Cr)原子比值分别为0.44～0.52和0.41～0.43,当其分别趋于0.44和0.41时,薄膜的显微硬度分别达到最大值3300HV_(0.01)和3600HV_(0.01),膜/基结合力也分别达到最大值190N和200N。(Ti,Al,Zr,Cr)N多元膜的摩擦磨损机理均为以塑性变形为主要特征的粘着磨损,并伴有轻微的磨粒磨损。在常温和高温条件下磨损时,平均摩擦系数在0.3～0.5之间。薄膜的摩擦系数曲线和磨损表面形貌分析表明,随着沉积偏压的增加,其耐磨性有所提高,而且硬质合金基体略优于高速钢基体上薄膜的耐磨性。另外,在短时氧化条件下,高速钢和硬质合金基体上的(Ti,Al,Zr,Cr)N膜分别在800℃和700℃时具有良好的抗高温氧化性能,在XRD谱中观察到了金红石结构的TiO_2;在长时氧化条件下,高速钢和硬质合金基体上(Ti,Al,Zr,Cr)N膜的抗高温循环氧化温度分别为700℃和600℃。
(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N多元双层膜具有比(Ti,Al,Zr,Cr)N单层膜更高的硬度和更强的膜/基结合力。当高速钢和硬质合金基体上(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N膜的(Al+Zr+Cr)/(Ti+Al+Zr+Cr)原子比值分别达到0.44和0.40时,薄膜的显微硬度分别达到最大值3450HV_(0.01)和4000HV_(0.01),膜/基结合力也分别达到最大值190N和＞200N。同时,(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜具有比(Ti,Al,Zr,Cr)N单层膜更优的耐磨损性能,其在常温和高温下磨损时的平均摩擦系数在0.3～0.35之间。而且,氧化增重、氧化膜的表面形貌及其相结构的分析表明,(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜具有比(Ti,Al,Zr,Cr)N单层膜更为良好的抗高温氧化性能。
CrN/(Ti,Al,Zr,Cr)N多元双层膜具有比(Ti,Al,Zr,Cr)N单层膜更高、但略低于(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜的硬度,同时具有比(Ti,Al,Zr,Cr)N单层膜和(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜都强的膜/基结合力。当高速钢和硬质合金基体上CrN/(Ti,Al,Zr,Cr)N膜的(Al+Zr+Cr)/(Ti+Al+Zr+Cr)原子比值分别趋于0.45和0.40时,薄膜的显微硬度分别达到最大值3400HV_(0.01)和3900HV_(0.01),膜/基结合力也分别达到最大值190N和＞200N。同时,CrN/(Ti,Al,Zr,Cr)N双层膜具有比(Ti,Al,Zr,Cr)N单层膜更优、但略低于(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N双层膜的耐磨损性能,其在常温和高温下磨损时的平均摩擦系数分别在0.3～0.4和0.3～0.45之间。而且,CrN/(Ti,Al,Zr,Cr)N双层膜具有比(Ti,Al,Zr,Cr)N单层膜更为良好的抗高温氧化性能。在短时氧化条件下,硬质合金基体上CrN/(Ti,Al,Zr,Cr)N膜的抗高温氧化温度进一步提高到800℃。
TiAlZrCr/(Ti,Al,Zr,Cr)N多元梯度膜具有比(Ti,Al,Zr,Cr)N单层膜及(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N和CrN/(Ti,Al,Zr,Cr)N双层膜更高的硬度和更强的膜/基结合力。当高速钢和硬质合金基体上梯度膜的(Al+Zr+Cr)/(Ti+Al+Zr+Cr)原子比值分别达到0.45和0.39时,薄膜的显微硬度分别达到最大值3500HV_(0.01)和4000HV_(0.01),膜/基结合力也分别达到最大值200N和＞200N。同时,TiAlZrCr/(Ti,Al,Zr,Cr)N梯度膜具有比(Ti,Al,Zr,Cr)N单层膜及(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N和CrN/(Ti,Al,Zr,Cr)N双层膜更优的耐磨性,其在常温和高温下磨损时的平均摩擦系数分别在0.25～0.3和0.3～0.35之间。而且,在短时氧化条件下,高速钢和硬质合金两种基体上的TiAlZrCr/(Ti,Al,Zr,Cr)N梯度膜在800℃时均具有良好的抗高温氧化性能;在长时氧化条件下,高速钢和硬质合金两种基体上TiAlZrCr/(Ti,Al,Zr,Cr)N梯度膜的抗高温循环氧化温度均为700℃,与(Ti,Al,Zr,Cr)N单层膜及(Ti,Al,Zr)N/(Ti,Al,Zr,Cr)N和CrN/(Ti,Al,Zr,Cr)N双层膜相比,其抗高温氧化性能得到了明显的改善。
The TiN hard films deposited on the cutting tools of high speed steel and cemented carbide can enhance their hardness and wear resistance, which, in turn, improve the cutting performance and service life. However, high speed cutting has been the main trend in the mechanical processing field. The TiN hard films deposited cutting tools would not fulfill the function requirements of the numerical controlled processing machines, which gradually become more popular. On the other hand, the various composite techniques, namely film alloying, multilayer and gradient-layer, could improve the comprehensive quality and service life of the hard films. Therefore, the objective of this study is to achieve the better properties of TiN-based composite films by adding the different alloy elements and modifying the film structures.
The two Ti-Al-Zr targets and one pure Cr target were used to prepare four types of Ti-Al-Zr-Cr-N composite hard films, namely (Ti, Al, Zr, Cr) N multi-component films, (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films, CrN/(Ti, Al, Zr, Cr) N bilayered films and TiAlZrCr/(Ti, Al, Zr, Cr) N gradient films, on the substrates of high speed steel (W18Cr4V) and cemented carbide (WC-8%Co). The composition, morphology, roughness and microstructure of the films were analyzed by energy disperse X-ray spectroscopy (EDS), scanning electron microscopy (SEM), laser scanning Confocal optical microscopy and X-ray diffraction (XRD). Vickers indentation and scratch test were performed to measure the micro-hardness and the adhesive strength between the film and the substrate. Meanwhile, the wear resistance of the films was studied by abrasion tester at the room temperature (15℃) and elevated temperature (500℃), and the worn surface morphologies were studied by SEM. Furthermore, short-term isothermal (at 600℃, 700℃, 800℃and 900℃for 4h) and long-term cyclic (at 700℃ and 800℃for 100h) high temperature oxidation behaviors of the films were studied, and the oxide scales formed on the film specimens were characterized by SEM, EDS and XRD.
It was showed that the obtained Ti-Al-Zr-Cr-N composite hard films were of the TiN (B1-NaCl) type face-centered cubic structure. The compositions of the four composite films did not change too much at the other bias voltages except at -50V. The surface morphologies of the composite films were isotropy and dense; however, there were many macro-particles (or micro-drops) and pores. By increasing the bias voltage, the drop contamination on the films decreased significantly, and then the surface roughness of the films was also improved. The cross-section morphologies revealed the typical and dense columnar structure. No evident defects were observed at the interface between the composite films and the substrates. The thickness of the four composite films was about l~1.5|xm at the different bias voltages, and decreased with increasing the bias voltage.
In the (Ti, Al, Zr, Cr) N multi-component films, the atomic ratio of (Al+Zr+Cr)/ (Ti+Al+Zr+Cr) varied from 0.44 to 0.52 on the W18Cr4V substrates, whereas it varied from 0.41 to 0.43 on the WC-8%Co substrates. When the atomic ratio approached 0.44 and 0.41, the micro-hardness of the films was improved up to 3300HV_(0.01) and 3600HV_(0.01), respectively. The adhesive strength between the film and the substrate was also enhanced up to 190N and 200N, respectively. The wear behavior of the films was characterized by the adhesive wear that was caused by the plastic deformation feature and the slight abrasive wear. The average values of friction coefficient varied between 0.3 and 0.5 at the room temperature and elevated temperature in the (Ti, Al, Zr, Cr) N multi-component films. The friction coefficient curves and the worn surface morphologies showed that the wear resistance was improved as the bias voltage increased. The properties of the films on the WC-8%Co substrates were better than those on the W18Cr4V substrates. Moreover, under short-term isothermal condition, the (Ti, Al, Zr, Cr) N films presented the excellent high temperature oxidation resistance on both the W18Cr4V (up to 800℃) and WC-8%Co (up to 700℃) substrates, and an oxide scale of TiO_2 was observed by XRD. On the other hand, under long-term cyclic high temperature condition, the oxidation resistant temperature of the (Ti, Al, Zr, Cr) N films was about 700℃on the W18Cr4V substrates and 600℃on the WC-8%Co substrates.
The micro-hardness of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films and the adhesive strength between the bilayered film and the substrate were increased remarkably with the addition of (Ti, Al, Zr) N interlayer. When the atomic ratio of (Al+Zr+Cr)/(Ti+Al+Zr+Cr) reached 0.44 on the W18Cr4V substrates and 0.40 on the WC-8%Co substrates, the micro-hardness of the films was improved up to 3450HV_(0.01) and 4000HV_(0.01), respectively. The adhesive strength between the film and the substrate was also enhanced to 190N and above 200N, respectively. Meanwhile, the wear resistance of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films was superior to those of the (Ti, Al, Zr, Cr) N single-layered films. The average values of friction coefficient varied between 0.3 and 0.35 at the room temperature and elevated temperature in the bilayered films. Moreover, the high temperature oxidation resistance of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films was improved with the addition of (Ti, Al, Zr) N interlayer according to the analysis of mass gain, morphology and microstructure of the oxide scales.
In the CrN/(Ti, Al, Zr, Cr) N bilayered films, the micro-hardness values were higher than those of the (Ti, Al, Zr, Cr) N single-layered films, but lower than those of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films. The CrN/(Ti, Al, Zr, Cr) N bilayered films also presented the superior adhesive strength, as compared with (Ti, Al, Zr, Cr) N and (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N films. When the atomic ratio of (Al+Zr+Cr) /(Ti+Al+Zr+Cr) reached 0.45 on the W18Cr4V substrates and 0.40 on the WC-8%Co substrates, the micro-hardness of the films was improved up to 34OOHV_(0.01) and 3900HV_(0.01), respectively. The adhesive strength between the film and the substrate was also enhanced up to 190N and above 200N, respectively. Meanwhile, the wear resistance of the CrN/(Ti, Al, Zr, Cr) N bilayered films was superior to those of the (Ti, Al, Zr, Cr) N single-layered films, while not as good as those of the (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N bilayered films. The average values of friction coefficient varied between 0.3 and 0.4 at the room temperature and varied between 0.3 and 0.45 at the elevated temperature in the CrN/(Ti, Al, Zr, Cr) N films. Moreover, the high temperature oxidation resistance of the CrN/(Ti, Al, Zr, Cr) N bilayered films was improved with the addition of CrN interlayer, in which the oxidation resistance temperature of the films on the WC-8%Co substrates was up to 800℃under the short-term isothermal oxidation condition.
The micro-hardness and adhesive strength of the TiAlZrCr/(Ti, Al, Zr, Cr) N gradient films were higher than those of the (Ti, Al, Zr, Cr) N, (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N and CrN/(Ti, Al, Zr, Cr) N films. When the atomic ratio of (Al+Zr+Cr)/(Ti +Al+Zr+Cr) approached 0.45 on the W18Cr4V substrates and 0.39 on the WC-8%Co substrates, the micro-hardness of the gradient films was enhanced up to 3500HV_(0.01) and 4000HV_(0.01), respectively. The adhesive strength between the gradient film and the substrate was also enhanced up to 200N and above 200N, respectively. Meanwhile, the wear resistance of the TiAlZrCr/(Ti, Al, Zr, Cr) N gradient films was superior to those of the (Ti, Al, Zr, Cr) N, (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N and CrN/(Ti, Al, Zr, Cr) N films. The average values of friction coefficient varied between 0.25 and 0.3 at the room temperature and varied between 0.3 and 0.35 at the elevated temperature in the gradient films. Moreover, under short-term isothermal condition, the high temperature oxidation resistance of the films was excellent up to 800℃on both the W18Cr4V and WC-8%Co substrates. Under long-term cyclic high temperature condition, the oxidation resistance of the films was excellent at about 700℃on both the W18Cr4V and WC-8%Co substrates. Therefore, the high temperature oxidation resistance of the TiAlZrCr/(Ti, Al, Zr, Cr) N gradient films was obviously improved and better than those of (Ti, Al, Zr, Cr) N, (Ti, Al, Zr) N/(Ti, Al, Zr, Cr) N and CrN/(Ti, Al, Zr, Cr) N films.
引文
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