稀土对CrAlTiN薄膜制备和性能的影响及机理研究
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摘要
由于硬质涂层刀具、模具的使用寿命远远高于一般的刀具、模具。因此,在生产企业使用硬质涂层刀具、模具已经非常普遍。同时,中国是一个稀土资源大国,将稀土元素引入刀具、模具涂层行业,发展稀土改性的硬质涂层不仅具有理论意义而且具有重要的实用价值。
本文采用英国Teer公司生产的UDP450磁控溅射机和Cr靶、Ti靶、Al靶、Al-Y0.26 wt.%靶、Al-Y0.84 wt.%靶、Al-Y1.48 wt.%靶、Al-Ce12 wt.%靶,通过改变氮气流量、负偏压沉积CrAlTi(Y)N薄膜和CrAlTi(Ce)N薄膜。在国际上首次研究了稀土元素在溅射过程中对溅射产额的影响;研究了基体QT700-2表面石墨球上的CrAlTi(Y)N薄膜失效机理;研究了Al-Y合金靶材中不同稀土Y含量对CrAlTi(Y)N薄膜的生长、相组成、成分、结构、粗糙度、硬度、结合强度的影响;研究了氮气流量、偏压对CrAlTi(Y)N薄膜和CrAlTi(Ce)N薄膜的生长、相组成、成分、结构、粗糙度、硬度及耐磨性的影响。
The hard coating tools, such as cutting tools and die, have been used in manufacturing because the hard coating can prolong the tools uselife. At the same time, China has enough resource of rare earth element. So we can introduce rare earth element into hard coating in order to get new one. As a result, it possesses not only theoretical significance but important practical value to study.
In this study UDP450 magnetron sputtering machine, Cr target, Ti target, Al target, Al-Y0.26 wt.% target, Al-Y0.84 wt.% target, Al-Y1.48 wt.% target and Al-Ce12 wt.% target were used to prepare CrAlTi(Y)N films and CrAlTi(Ce)N films. It is the first time to study the effect of rare earth element on sputtering yield during the sputtering process. The failure process of CrAlTi(Y)N film on the graphite of QT700-2 and the effect of Y content in Al-Y target on the CrAlTi(Y)N film depositing, phase composition, structure, roughness, hardness and binding force were also studied. It was studied that the effects of N2 flow and bias voltage on the CrAlTi(Y)N film and CrAlTi(Ce)N film depositing, phase composition, structure, roughness, hardness, friction and wear. The results were as follows:
1. Effect of Y content in Al-Y target on the sputtering yield of Al, and effect of Ce on the sputtering process under different bias voltages were studied. According to the experiment results, the relationship of sputtering yield Y was expressed as following:
Impact factorαis about rare earth element content; impact factorγis about the energy of sputtering ions.
2. CrAlTi(Y)N film invalidation on graphite of QT700-2 was studied. The failure mode of CrAlTi(Y)N film included three courses: CrAlTi(Y)N film cracked; CrAlTi(Y)N film failure; graphite exposed. The shiver of CrAlTi(Y)N promot the process of friction and wear.
3. According to the present experimental results: The deposition speed of CrAlTi(Y)N film increased with the increasing of Y content in Al-Y target. Al content in CrAlTi(Y)N film increased with the increasing of Y content in Al-Y target, and Cr content decreased. The roughness of CrAlTi(Y)N film is decreased as increasing of Y content in Al-Y target. The grain size of CrAlTi(Y)N film decreased with the increasing of Y content in Al-Y target. The hardness of CrAlTi(Y)N film decreased with the increasing of Y content in Al-Y target. As Y content is 0.84%, the hardness of CrAlTi(Y)N film is the smallest. The plasticity and binding force of CrAlTi(Y)N film increased with the increasing of Y content in Al-Y target.
4、According to the present experimental results: The deposition speed of CrAlTi(Y)N film decreased with the increasing of N2 flow. XRD diffraction peak of CrAlTi(Y)N film changed as changing N2 flow. When OEM is 46, (200) decreased, (220) and (311) increased. The roughness of CrAlTi(Y)N film is decreased as increasing N2 flow. As OEM is 32, the roughness of CrAlTi(Y)N film is the smallest. The grain size of CrAlTi(Y)N film is almost not changed with the increasing of N2 flow. When OEM is 24, there is not column structure in CrAlTi(Y)N film. The hardness of CrAlTi(Y)N film increased with the increasing of N2 flow.
5、According to the present experimental results: The deposition speed of CrAlTi(Y)N film decreased with the increasing of bias voltage. XRD diffraction peak of CrAlTi(Y)N film is changed as increasing bias voltage, and the crystal preferred orientation of CrAlTi(Y)N film is (200). The roughness of CrAlTi(Y)N film decreased with the increasing of bias voltage. When bias voltage is 100V, the roughness of CrAlTi(Y)N film is the smallest. The grain size of CrAlTi(Y)N film decreased with the increasing of bias voltage. When bias voltage is 120V, the structure of CrAlTi(Y)N film is not column structure. The hardness of CrAlTi(Y)N film increased with the increasing of bias voltage.
6、According to the friction and wear experimental results:
(1)The friction coefficient of CrAlTi(Y)N film which prepared by change N2 flow and bias voltage is 0.4-0.55.
(2) CrAlTi(Y)N film depositing on the steel could increase the friction and wear properties notably. Wear mass loss of CrAlTi(Y)N film depositing on T10A increases with the increasing of Y content in Al-Y target, increases with the increasing of bias voltage, increases with the increasing of N2 flow.
(3)The effects of bias voltage and N2 flow on the friction and wear of CrAlTi(Y)N film are not regular as the substrate is QT700-2. The mechanism is attributed to the graphite pebbles. The effect of graphite pebbles is more notable than the effect of Y content in Al-Y target, bias voltage and N2 flow.
7. According to the present experimental results: The deposition speed of CrAlTi(Ce)N film decreased with the increasing of N2 flow. The crystal preferred orientation of CrAlTi(Ce)N film is (111), (200) decreased with the increasing of OEM. The roughness of CrAlTi(Ce)N film decreased with the increasing of N2 flow. The grain size of CrAlTi(Ce)N film almost not changed with the increasing of N2 flow. The hardness of CrAlTi(Ce)N film increased with the increasing of N2 flow.
8. According to the present experimental results: The deposition speed of CrAlTi(Ce)N film decreased with the increasing of bias voltage. The crystal preferred orientation of CrAlTi(Ce)N film is (111) with the increasing of bias voltage from 60V to 100V. When bias voltage is 120V, there is amorphous. The roughness of CrAlTi(Ce)film decreased with the increasing of bias voltage. The grain size of CrAlTi(Ce) film decreased with the increasing of bias voltage. When bias voltage is 120V, the structure of CrAlTi(Ce)N film is amorphous, there are many crater-shapes on the surface of CrAlTi(Ce)N film. The hardness of CrAlTi(Ce)N film increased with the increasing of bias voltage. When bias voltage is 120V, the hardness decreased.
9. According to the friction and Wear experimental results:
(1) Wear resistance of CrAlTi(Ce)N film depositing on Cr12MoV rise as increasing bias voltage.
(2) Wear mass loss of CrAlTi(Ce)N film deposited on Cr12MoV matrix material increased with the increasing of N2 flow.
(3) The effects of bias voltage and N2 flow on the friction and wear of CrAlTi(Ce)N film are not regular as the substrate is QT700-2. The mechanism is attributed to the graphite pebbles.
本文采用英国Teer公司生产的UDP450磁控溅射机和Cr靶、Ti靶、Al靶、Al-Y0.26 wt.%靶、Al-Y0.84 wt.%靶、Al-Y1.48 wt.%靶、Al-Ce12 wt.%靶,通过改变氮气流量、负偏压沉积CrAlTi(Y)N薄膜和CrAlTi(Ce)N薄膜。在国际上首次研究了稀土元素在溅射过程中对溅射产额的影响;研究了基体QT700-2表面石墨球上的CrAlTi(Y)N薄膜失效机理;研究了Al-Y合金靶材中不同稀土Y含量对CrAlTi(Y)N薄膜的生长、相组成、成分、结构、粗糙度、硬度、结合强度的影响;研究了氮气流量、偏压对CrAlTi(Y)N薄膜和CrAlTi(Ce)N薄膜的生长、相组成、成分、结构、粗糙度、硬度及耐磨性的影响。
The hard coating tools, such as cutting tools and die, have been used in manufacturing because the hard coating can prolong the tools uselife. At the same time, China has enough resource of rare earth element. So we can introduce rare earth element into hard coating in order to get new one. As a result, it possesses not only theoretical significance but important practical value to study.
In this study UDP450 magnetron sputtering machine, Cr target, Ti target, Al target, Al-Y0.26 wt.% target, Al-Y0.84 wt.% target, Al-Y1.48 wt.% target and Al-Ce12 wt.% target were used to prepare CrAlTi(Y)N films and CrAlTi(Ce)N films. It is the first time to study the effect of rare earth element on sputtering yield during the sputtering process. The failure process of CrAlTi(Y)N film on the graphite of QT700-2 and the effect of Y content in Al-Y target on the CrAlTi(Y)N film depositing, phase composition, structure, roughness, hardness and binding force were also studied. It was studied that the effects of N2 flow and bias voltage on the CrAlTi(Y)N film and CrAlTi(Ce)N film depositing, phase composition, structure, roughness, hardness, friction and wear. The results were as follows:
1. Effect of Y content in Al-Y target on the sputtering yield of Al, and effect of Ce on the sputtering process under different bias voltages were studied. According to the experiment results, the relationship of sputtering yield Y was expressed as following:
Impact factorαis about rare earth element content; impact factorγis about the energy of sputtering ions.
2. CrAlTi(Y)N film invalidation on graphite of QT700-2 was studied. The failure mode of CrAlTi(Y)N film included three courses: CrAlTi(Y)N film cracked; CrAlTi(Y)N film failure; graphite exposed. The shiver of CrAlTi(Y)N promot the process of friction and wear.
3. According to the present experimental results: The deposition speed of CrAlTi(Y)N film increased with the increasing of Y content in Al-Y target. Al content in CrAlTi(Y)N film increased with the increasing of Y content in Al-Y target, and Cr content decreased. The roughness of CrAlTi(Y)N film is decreased as increasing of Y content in Al-Y target. The grain size of CrAlTi(Y)N film decreased with the increasing of Y content in Al-Y target. The hardness of CrAlTi(Y)N film decreased with the increasing of Y content in Al-Y target. As Y content is 0.84%, the hardness of CrAlTi(Y)N film is the smallest. The plasticity and binding force of CrAlTi(Y)N film increased with the increasing of Y content in Al-Y target.
4、According to the present experimental results: The deposition speed of CrAlTi(Y)N film decreased with the increasing of N2 flow. XRD diffraction peak of CrAlTi(Y)N film changed as changing N2 flow. When OEM is 46, (200) decreased, (220) and (311) increased. The roughness of CrAlTi(Y)N film is decreased as increasing N2 flow. As OEM is 32, the roughness of CrAlTi(Y)N film is the smallest. The grain size of CrAlTi(Y)N film is almost not changed with the increasing of N2 flow. When OEM is 24, there is not column structure in CrAlTi(Y)N film. The hardness of CrAlTi(Y)N film increased with the increasing of N2 flow.
5、According to the present experimental results: The deposition speed of CrAlTi(Y)N film decreased with the increasing of bias voltage. XRD diffraction peak of CrAlTi(Y)N film is changed as increasing bias voltage, and the crystal preferred orientation of CrAlTi(Y)N film is (200). The roughness of CrAlTi(Y)N film decreased with the increasing of bias voltage. When bias voltage is 100V, the roughness of CrAlTi(Y)N film is the smallest. The grain size of CrAlTi(Y)N film decreased with the increasing of bias voltage. When bias voltage is 120V, the structure of CrAlTi(Y)N film is not column structure. The hardness of CrAlTi(Y)N film increased with the increasing of bias voltage.
6、According to the friction and wear experimental results:
(1)The friction coefficient of CrAlTi(Y)N film which prepared by change N2 flow and bias voltage is 0.4-0.55.
(2) CrAlTi(Y)N film depositing on the steel could increase the friction and wear properties notably. Wear mass loss of CrAlTi(Y)N film depositing on T10A increases with the increasing of Y content in Al-Y target, increases with the increasing of bias voltage, increases with the increasing of N2 flow.
(3)The effects of bias voltage and N2 flow on the friction and wear of CrAlTi(Y)N film are not regular as the substrate is QT700-2. The mechanism is attributed to the graphite pebbles. The effect of graphite pebbles is more notable than the effect of Y content in Al-Y target, bias voltage and N2 flow.
7. According to the present experimental results: The deposition speed of CrAlTi(Ce)N film decreased with the increasing of N2 flow. The crystal preferred orientation of CrAlTi(Ce)N film is (111), (200) decreased with the increasing of OEM. The roughness of CrAlTi(Ce)N film decreased with the increasing of N2 flow. The grain size of CrAlTi(Ce)N film almost not changed with the increasing of N2 flow. The hardness of CrAlTi(Ce)N film increased with the increasing of N2 flow.
8. According to the present experimental results: The deposition speed of CrAlTi(Ce)N film decreased with the increasing of bias voltage. The crystal preferred orientation of CrAlTi(Ce)N film is (111) with the increasing of bias voltage from 60V to 100V. When bias voltage is 120V, there is amorphous. The roughness of CrAlTi(Ce)film decreased with the increasing of bias voltage. The grain size of CrAlTi(Ce) film decreased with the increasing of bias voltage. When bias voltage is 120V, the structure of CrAlTi(Ce)N film is amorphous, there are many crater-shapes on the surface of CrAlTi(Ce)N film. The hardness of CrAlTi(Ce)N film increased with the increasing of bias voltage. When bias voltage is 120V, the hardness decreased.
9. According to the friction and Wear experimental results:
(1) Wear resistance of CrAlTi(Ce)N film depositing on Cr12MoV rise as increasing bias voltage.
(2) Wear mass loss of CrAlTi(Ce)N film deposited on Cr12MoV matrix material increased with the increasing of N2 flow.
(3) The effects of bias voltage and N2 flow on the friction and wear of CrAlTi(Ce)N film are not regular as the substrate is QT700-2. The mechanism is attributed to the graphite pebbles.
引文
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