非晶Al-Mg-B超硬薄膜材料制备与性能研究
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摘要
随着现代制造业的快速发展,人们对切削刀具、磨具及耐磨零部件的硬度、耐磨性和使用寿命等性能提出了更高的要求。因此,超硬材料逐渐向低密度、低摩擦系数、低成本等方向发展。由于硼化物材料具高硬度和低摩擦系数等特性,在切、磨工具应用上都有着优异的表现。因此,超硬硼化物材料的研究与开发受到了各国研究人员的重视。
在硼化物材料中,三元金属硼化物AlMgB14因其具有高硬度、低摩擦系数等优点而备受关注。前人通常采用粉末高温烧结方法制备大块晶体材料并予以使用。近年来,薄膜材料因为具有用量少、可附着在形状复杂的工具表面并能赋予基体新特性等优点,在国民经济的诸多领域中发挥着重要的作用。另一方面,非晶材料通常具有高强度、高韧性和极强的耐腐性能等特点,可在环境复杂及恶劣的条件下稳定工作。因此,制备非晶Al-Mg-B薄膜材料,不仅可以进一步提高该材料的使用性能,还将在三元系金属硼化物(XYB14)的研究和开发方面取得突破性进展。然而,至今缺乏对高性能非晶Al-Mg-B薄膜材料的制备和硬化机理的研究,从而制约了非晶Al-Mg-B薄膜材料性能的提升,影响了该材料的进一步开发与应用。
针对这个问题,本论文使用磁控溅射镀膜系统,采用多靶共溅射方法,以提高非晶Al-Mg-B薄膜材料的力学性能为目的,分别对薄膜的制备工艺(溅射功率、沉积温度、沉积气压及负偏压)进行优化,并对影响薄膜性能的关键工艺参数进行分析。研究发现,随硼靶溅射功率的增大,薄膜内硼元素含量逐渐增多,薄膜硬度呈先上升后下降的变化趋势,薄膜摩擦系数却一直在逐渐减小；随着薄膜制备沉积温度和沉积气压的升高,薄膜硬度也随之增大,同时其摩擦系数在逐渐减小；随着负偏压的增大,薄膜硬度呈先上升后下降的变化趋势。在成分优化方面,室温下制备非晶A1-Mg-B薄膜,当硼含量约为93.1at.%时,薄膜具有最高硬度(37.1GPa),此时摩擦系数也仅为0.15。而具有近似晶体成分的Al-Mg-B薄膜其硬度为31.1GPa,与晶体AlMgB14(28GPa)材料相当。对于具有近似晶体成分的Al-Mg-B非晶薄膜,其优化的制备工艺为沉积温度600℃、沉积气压0.9Pa、沉积负偏压80V。
在此基础上,应用优化的薄膜制备工艺参数,在YG6X硬质合金刀具(20GPa-30GPa)表面沉积制备非晶Al-Mg-B薄膜,该薄膜与硬质合金具有很好的结合强度。制备的涂层刀具拥有44.6GPa的高硬度和0.11的低摩擦系数。与未涂层刀具相比,其切削性能得到明显提高。
在非晶Al-Mg-B薄膜成功制备基础上,本论文对非晶Al-Mg-B材料的硬化机理进行了分析,提出非晶Al-Mg-B薄膜中保留了晶体材料中的B12二十面体的短程有序结构,这个结构对非晶薄膜的硬度有决定性影响。这一结论首先通过第一性原理计算AlMgB14和α-B的维氏硬度,从电子结构角度阐明了B12二十面体是决定AlMgB14材料具有高硬度的主要因素。随后,通过元素掺杂非晶Al-Mg-B薄膜,发现Ti、Si元素掺杂后的非晶Al-Mg-B薄膜仍具有较高的硬度,且B12二十面体依然稳定存在,但Cr、N元素掺杂却阻碍(或破坏)薄膜内B12二十面体的形成及稳定存在,进而降低了薄膜的力学性能。这一结果验证了B12二十面体在非晶薄膜高硬度性质中的作用。
基于B12二十面体在非晶薄膜高硬度性质中的作用,通过掺杂选择能够稳定B12二十面体结构的新元素种类,进而应用[团簇](连接原子)结构模型,可以实现开发具有更高性能的新型金属硼化物。
本论文研究结果为Al-Mg-B (?)非晶薄膜涂层刀具提供制备工艺参考,还可推动新型硼化物的研究与开发。
With the rapid development of modern manufacturing industry, higher properties are requested for cutting tools, grinding tools and wear parts, such as the higher hardness, the better wearing resistance, the longer service life. Therefore, super-hard materials are gradually developed to achieve low density, low friction coefficient, low cost et al. Due to the boride material possesses excellent hardness and wearing resistance, it shows excellent performance as the production of cutting tools and grinding tools. Consequently, the research and development of super-hard boride material have attracted much attention.
In boride material, ternary metal boride AlMgB14has beed widely investigated due to its advantages of high hardness and low friction coefficient. Bulk crystalline materials prepared by high-temperature sintering of powder are generally used in previous investigation. However, in practical application, the thin film material plays an important role in the national economy in many fields. This is because the thin films can be attached to the surface of the complex tools by using fewer amounts and consequently endued the substrate material with new properties. On the other hand, due to the characteristics of high strength, high toughness and strong corrosion resistance of the amorphous materials, it has the good performance in many complex and harsh work environment. Therefore, amorphous Al-Mg-B thin film can further improve the performance, and promote the research and development of ternary metal boride (XYB14). However, the study of deposition process and hardening mechanism is still lack, which constrains performance optimization of the amorphous Al-Mg-B thin film materials and further development and application.
To address this problem, in this present work, the magnetron sputtering technology and multi-target sputtering scheme are employed to prepare amorphous Al-Mg-B thin films. The process parameters, including the sputtering power, deposition temperature, deposition pressure and negative bias, were optimized. The critical proress parameters which could affect the film properties were analyzed. It was found out that the hardness of the films increases at first and then decrease with the increase in boron sputtering power but the surface roughness and friction coefficient of the film decreased gradually; the hardness of the film increased and the friction coefficient decreased with the increase in deposition temperature and deposition pressure; the hardness of films increased firstly and then decreased with the increase in negative bias. In the case of composition optimization, the highest hardness37.1GPa appeares at a composition of boron93.1at.%, while the friction coefficient was only0.15. On the other hand, amorphous Al-Mg-B thin film with a similar composition as that of crystalline AlMgB]4material has a comparative hardness comparing with crystal AlMgB14material (28GPa), the nano-hardness was31.1GPa. Moreover, the optimized deposition conditions corresponding to this film are deposition temperature600℃, deposition pressure0.9Pa. and negative bias voltage80V.
Based on these results, high performance Al-Mg-B amorphous films were deposited on the surface of YG6X cemented carbide cutting tools by applying these optimized deposition conditions. The film shows relatively high bond strength with the YG6X alloy. The hardness of YG6X was44.6GPa and the friction coefficients was0.11. Moreover, he coated cutting tool shows better cutting performance.
According to the deposition and characterization results, the hardening mechanism of Al-Mg-B amorphous film was analyzed. It was suggested that the short-range orderd Bl2icosahedron structure in the crystalline materials was reserved in the amorphous film, and the existence of this structure dominantes the hardness of the amorphous film. This suggestion was first demonstrated by first principle simulation of the hardness of AlMgB14and a-B. The determinant effect of B12icosahedron structure on the hardness was elucidated by electronic structure simulation. Then, the Al-Mg-B amorphous films were doped by four different elements. It was found out that the amorphous Al-Mg-B films doped by Ti and Si still have a high hardness, and B12icosahedron still exists with a steady state. However, the doping of Cr and N blocked or damaged the formation and existence of B12icosahedron, and. hence, the mechanical performance of Al-Mg-B films was decreased. This result further confirms the role of B12icosahedron structure in the high hardness of Al-Mg-B amorphous films.
According to the effect of B12icosahedron structure on the high hardness of Al-Mg-B amorphous films, elements that can stabilized the B12icosahedron structure can be selected by doping. Then, a [cluster](connecting atoms) model can be used for developing new metal borides materials with high performance.
The results of this work provide a reference of deposition proress for industrial manufacture of coated cutting tools. Moreover, they can promote the development of new metal borides materials with high performance.
在硼化物材料中,三元金属硼化物AlMgB14因其具有高硬度、低摩擦系数等优点而备受关注。前人通常采用粉末高温烧结方法制备大块晶体材料并予以使用。近年来,薄膜材料因为具有用量少、可附着在形状复杂的工具表面并能赋予基体新特性等优点,在国民经济的诸多领域中发挥着重要的作用。另一方面,非晶材料通常具有高强度、高韧性和极强的耐腐性能等特点,可在环境复杂及恶劣的条件下稳定工作。因此,制备非晶Al-Mg-B薄膜材料,不仅可以进一步提高该材料的使用性能,还将在三元系金属硼化物(XYB14)的研究和开发方面取得突破性进展。然而,至今缺乏对高性能非晶Al-Mg-B薄膜材料的制备和硬化机理的研究,从而制约了非晶Al-Mg-B薄膜材料性能的提升,影响了该材料的进一步开发与应用。
针对这个问题,本论文使用磁控溅射镀膜系统,采用多靶共溅射方法,以提高非晶Al-Mg-B薄膜材料的力学性能为目的,分别对薄膜的制备工艺(溅射功率、沉积温度、沉积气压及负偏压)进行优化,并对影响薄膜性能的关键工艺参数进行分析。研究发现,随硼靶溅射功率的增大,薄膜内硼元素含量逐渐增多,薄膜硬度呈先上升后下降的变化趋势,薄膜摩擦系数却一直在逐渐减小；随着薄膜制备沉积温度和沉积气压的升高,薄膜硬度也随之增大,同时其摩擦系数在逐渐减小；随着负偏压的增大,薄膜硬度呈先上升后下降的变化趋势。在成分优化方面,室温下制备非晶A1-Mg-B薄膜,当硼含量约为93.1at.%时,薄膜具有最高硬度(37.1GPa),此时摩擦系数也仅为0.15。而具有近似晶体成分的Al-Mg-B薄膜其硬度为31.1GPa,与晶体AlMgB14(28GPa)材料相当。对于具有近似晶体成分的Al-Mg-B非晶薄膜,其优化的制备工艺为沉积温度600℃、沉积气压0.9Pa、沉积负偏压80V。
在此基础上,应用优化的薄膜制备工艺参数,在YG6X硬质合金刀具(20GPa-30GPa)表面沉积制备非晶Al-Mg-B薄膜,该薄膜与硬质合金具有很好的结合强度。制备的涂层刀具拥有44.6GPa的高硬度和0.11的低摩擦系数。与未涂层刀具相比,其切削性能得到明显提高。
在非晶Al-Mg-B薄膜成功制备基础上,本论文对非晶Al-Mg-B材料的硬化机理进行了分析,提出非晶Al-Mg-B薄膜中保留了晶体材料中的B12二十面体的短程有序结构,这个结构对非晶薄膜的硬度有决定性影响。这一结论首先通过第一性原理计算AlMgB14和α-B的维氏硬度,从电子结构角度阐明了B12二十面体是决定AlMgB14材料具有高硬度的主要因素。随后,通过元素掺杂非晶Al-Mg-B薄膜,发现Ti、Si元素掺杂后的非晶Al-Mg-B薄膜仍具有较高的硬度,且B12二十面体依然稳定存在,但Cr、N元素掺杂却阻碍(或破坏)薄膜内B12二十面体的形成及稳定存在,进而降低了薄膜的力学性能。这一结果验证了B12二十面体在非晶薄膜高硬度性质中的作用。
基于B12二十面体在非晶薄膜高硬度性质中的作用,通过掺杂选择能够稳定B12二十面体结构的新元素种类,进而应用[团簇](连接原子)结构模型,可以实现开发具有更高性能的新型金属硼化物。
本论文研究结果为Al-Mg-B (?)非晶薄膜涂层刀具提供制备工艺参考,还可推动新型硼化物的研究与开发。
With the rapid development of modern manufacturing industry, higher properties are requested for cutting tools, grinding tools and wear parts, such as the higher hardness, the better wearing resistance, the longer service life. Therefore, super-hard materials are gradually developed to achieve low density, low friction coefficient, low cost et al. Due to the boride material possesses excellent hardness and wearing resistance, it shows excellent performance as the production of cutting tools and grinding tools. Consequently, the research and development of super-hard boride material have attracted much attention.
In boride material, ternary metal boride AlMgB14has beed widely investigated due to its advantages of high hardness and low friction coefficient. Bulk crystalline materials prepared by high-temperature sintering of powder are generally used in previous investigation. However, in practical application, the thin film material plays an important role in the national economy in many fields. This is because the thin films can be attached to the surface of the complex tools by using fewer amounts and consequently endued the substrate material with new properties. On the other hand, due to the characteristics of high strength, high toughness and strong corrosion resistance of the amorphous materials, it has the good performance in many complex and harsh work environment. Therefore, amorphous Al-Mg-B thin film can further improve the performance, and promote the research and development of ternary metal boride (XYB14). However, the study of deposition process and hardening mechanism is still lack, which constrains performance optimization of the amorphous Al-Mg-B thin film materials and further development and application.
To address this problem, in this present work, the magnetron sputtering technology and multi-target sputtering scheme are employed to prepare amorphous Al-Mg-B thin films. The process parameters, including the sputtering power, deposition temperature, deposition pressure and negative bias, were optimized. The critical proress parameters which could affect the film properties were analyzed. It was found out that the hardness of the films increases at first and then decrease with the increase in boron sputtering power but the surface roughness and friction coefficient of the film decreased gradually; the hardness of the film increased and the friction coefficient decreased with the increase in deposition temperature and deposition pressure; the hardness of films increased firstly and then decreased with the increase in negative bias. In the case of composition optimization, the highest hardness37.1GPa appeares at a composition of boron93.1at.%, while the friction coefficient was only0.15. On the other hand, amorphous Al-Mg-B thin film with a similar composition as that of crystalline AlMgB]4material has a comparative hardness comparing with crystal AlMgB14material (28GPa), the nano-hardness was31.1GPa. Moreover, the optimized deposition conditions corresponding to this film are deposition temperature600℃, deposition pressure0.9Pa. and negative bias voltage80V.
Based on these results, high performance Al-Mg-B amorphous films were deposited on the surface of YG6X cemented carbide cutting tools by applying these optimized deposition conditions. The film shows relatively high bond strength with the YG6X alloy. The hardness of YG6X was44.6GPa and the friction coefficients was0.11. Moreover, he coated cutting tool shows better cutting performance.
According to the deposition and characterization results, the hardening mechanism of Al-Mg-B amorphous film was analyzed. It was suggested that the short-range orderd Bl2icosahedron structure in the crystalline materials was reserved in the amorphous film, and the existence of this structure dominantes the hardness of the amorphous film. This suggestion was first demonstrated by first principle simulation of the hardness of AlMgB14and a-B. The determinant effect of B12icosahedron structure on the hardness was elucidated by electronic structure simulation. Then, the Al-Mg-B amorphous films were doped by four different elements. It was found out that the amorphous Al-Mg-B films doped by Ti and Si still have a high hardness, and B12icosahedron still exists with a steady state. However, the doping of Cr and N blocked or damaged the formation and existence of B12icosahedron, and. hence, the mechanical performance of Al-Mg-B films was decreased. This result further confirms the role of B12icosahedron structure in the high hardness of Al-Mg-B amorphous films.
According to the effect of B12icosahedron structure on the high hardness of Al-Mg-B amorphous films, elements that can stabilized the B12icosahedron structure can be selected by doping. Then, a [cluster](connecting atoms) model can be used for developing new metal borides materials with high performance.
The results of this work provide a reference of deposition proress for industrial manufacture of coated cutting tools. Moreover, they can promote the development of new metal borides materials with high performance.
引文
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