高密度硬盘磁头用超薄类金刚石薄膜的研究
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摘要
随着磁存储硬盘技术的不断发展,超薄类金刚石薄膜(DLC)的研究越来越成为材料领域的研究热点。本文分别采用Electron cyclotron resonance chemical vapor deposition (ECR-CVD电子回旋共振增强化学气相沉积)、Ion beam deposition optimization (IBO离子束辅助沉积技术)、Filtered cathodic vacuum arc (FCVA过滤阴极真空电弧技术)方法制备出Diamond-like carbon (DLC类金刚石)薄膜,主要以Vis(514nm) & UV(244nm) Raman对薄膜的结构分析为主线,从而反映薄膜的性能,具体见下。
首先研究了不同工艺制备的不同厚度薄膜的结构的变化。研究表明,ECR-CVD、IBO制备的a-C:H薄膜的生长主要分为两个阶段,50?以前,采用岛状生长;50?以后,采用平面层状生长,结构趋于稳定。而对于FCVA所制的ta-C薄膜,主要分三个阶段,第一阶段<15?:以岛状生长模式为主;第二阶段15~50?:以外延式的平面层状生长;第三阶段>50?:总体上属于纯粹的平面式生长,在微区部分,由于薄膜趋向于形成更多的四面体结构,属于岛状生长。此外,对于薄膜的硬度和密度比较,FCVA>IBO>CVD。因此,当厚度大于15?时,ta-C薄膜就开始变得致密、连续,可以达到耐磨性的要求,成为高密度磁头保护膜的首要选择。
在ECR-CVD方法中,采用CH4和N2混合气体制备a-C:H:N薄膜。研究表明,N的掺入,将使得薄膜的sp~3含量降低,以至硬度和密度降低。这是由于在a-C:H:N薄膜中,并没有形成大量的比金刚石结构更硬的C_3N_4 (C≡N)相,主要形成了C-N键。因此,氮掺杂并不能使a-C:H薄膜满足硬盘要求。
在FCVA方法中,对70nm厚膜分析发现,当倾斜衬底角度增加时,ta-C薄膜中的sp~3含量降低,同时薄膜中的sp2团簇的振动更加有序,使得内应力将比硬度下降的更快。对2nm薄膜拉曼分析表明,当倾斜衬底增加时,其内应力和硬度也会下降。这是由于当衬底倾斜时,入射离子形成平行于衬底表面的动量,不仅降低薄膜的sp~3相的形成,而且促使sp2相更加有序。
在FCVA方法中,对衬底偏压的研究表明,与70nm厚膜偏压效应相反,首次发现对2nm薄膜来说,当衬底偏压增加时,sp~3含量几乎在线性降低,对应的硬度也降低。这是因为偏压可以诱导与衬底形成更多的混合键,这些混合键都比C-C键长,故降低了薄膜的硬度;而对于厚膜来讲,界面混合层的影响可以忽略不计,高能量入射离子导致较多的sp~3键的过程占主导作用。
对于磁头使用的多层材料,DLC薄膜在AlTiC上沉积时,sp~3含量最高,对应硬度最高;而在FeCo、FeNi上,薄膜中的sp~3含量较低;在Au上,sp~3含量最低。
最后,为有效评估DLC在纳米级Lead区域结合力建立了超声震荡加化学腐蚀的方法。发现薄膜在AuCu上的结合力强于Au。从而对于可能由于DLC/ Lead间弱的结合力而引起的磁阻材料氧化问题,本实验结果提供了一种方法,从Wafer设计层面上,通过AuCu取代Au作为lead材料加以研究解决。
With the development of magnetic disk drive technology, ultra-thin diamond-like carbon (DLC) films have attracted considerable interest as a protective overcoat. In this thesis, firstly, DLC films are deposited using electron cyclotron resonance (ECR) chemical vapor deposition、ion beam deposition optimization (IBO) and filtered cathodic vacuum arc (FCVA) techniques, respectively. Then we consider in detail the use of a combined study of Raman spectra taken at two wavelengths (514 and 244 nm) to study the structure of films that can reflect its properties, and this is highlight part of the thesis. In addition, we propose a method for ultra-thin DLC films adherence evaluation on the nano-scale lead area of magnetic recording slider. The details are as following:
Firstly DLC films of different thickness from 10? to 100? are prepared by ECR-CVD、IBO and FCVA techniques, respectively. Through Raman spectroscopy study, the growth model for three kinds of films was discussed. For a-C:H films by ECR-CVD and IBO, its formation process mainly includes two stages. When film thickness is less than 50?, the carbon ions will form multiple nucleation centers like island, and when thickness is over 50?, the films developed with layer model and its structure became stable. But for ta-C films by FCVA, its growth process includes three stages. At the first stage, the thickness is less than 15? and it developed with island-like model. At the second stage, the thickness is from 15? to 50?, it developed with layer-like model and it already became stable. For the third stage, the thickness is over 50?, in mass area it could be described by layer model, while in local area it is with island model to form a little more tetrahedral structure. Thus, ta-C films of thickness over 15 ? already became dense and continuous and it will be the best choice for application of films in magnetic recording slider.
By ECR-CVD with a mixed gas of CH4 and N_2, the structure and mechanical properties of the a-C:H:N films are studied. The results show that a-C:H:N films with higher N content will contain less sp~3 sites. Hardness test of films confirmed that more N content corresponds to lower hardness. It also indicates that hard C≡N bond with high energy state is difficult to be formed by plasma doping, and additional N can not improve mechanical properties for a-C:H.
The tetrahedral amorphous carbon (ta-C) films by FCVA have been studied as a function of oblique angles of substrates varied from 0 to 60o, while keeping the energy of incident particles stable. The films contain less sp~3 sites and more ordered sp2 clustering as the substrate tilting for thicker films of 70 nm, and also a decrease of sp~3 content of ultra-thin films of 2 nm. Also it was found that the tilting can dramatically lower internal stress with less influence on hardness because hardness is related to sp~3 content, while internal stress is not only related to sp~3 content but also related to the order of sp2 cluster.
Additionally, substrate bias effect on ta-C film is studied. We found that the sp~3 content of 70 nm films increases with higher bias, while sp~3 content of 2 nm ultra-thin films falls almost linearly with bias. This is because substrate bias enhances mixing between the carbon films and substrate, and these mixing bonds are longer than C-C bonds. But for thicker films, the effect of mixing layer can be negligible compared to bias with higher carbon ion energy.
The sliders are composed of multi-layers which are mainly Fe-Co (Fe: 67%at, Co: 33%at) alloy, Fe-Ni (Fe: 18%at, Ni: 82%at) alloy, Au and Al_2O_3-TiC (Al_2O_3: 64%at, TiC: 36%at). The spectra show that the films deposited on Al_2O_3-TiC contains the highest sp~3 content, less sp~3 content on Fe-Co and Fe-Ni alloy, and the lowest of sp~3 content on Au substrate. It also indicates that the sequence of the anti-wear performance of ta-C film on different substrates is Al_2O_3-TiC > Fe-Co and Fe-Ni alloy > Au.
Finally, we propose a method with ultra-sonic plus chemical etching test, for ultra-thin Si/DLC films adherence evaluation on the nano-scale lead area of magnetic recording slider. The adherences of films on both Au and Au-Cu (Au: 93%at, Cu: 7%at) based lead are compared, and the results show Au-Cu lead exhibits better adhesion to Si/DLC than that with Au as confirmed by nano-scratch tests from the wafer level.
首先研究了不同工艺制备的不同厚度薄膜的结构的变化。研究表明,ECR-CVD、IBO制备的a-C:H薄膜的生长主要分为两个阶段,50?以前,采用岛状生长;50?以后,采用平面层状生长,结构趋于稳定。而对于FCVA所制的ta-C薄膜,主要分三个阶段,第一阶段<15?:以岛状生长模式为主;第二阶段15~50?:以外延式的平面层状生长;第三阶段>50?:总体上属于纯粹的平面式生长,在微区部分,由于薄膜趋向于形成更多的四面体结构,属于岛状生长。此外,对于薄膜的硬度和密度比较,FCVA>IBO>CVD。因此,当厚度大于15?时,ta-C薄膜就开始变得致密、连续,可以达到耐磨性的要求,成为高密度磁头保护膜的首要选择。
在ECR-CVD方法中,采用CH4和N2混合气体制备a-C:H:N薄膜。研究表明,N的掺入,将使得薄膜的sp~3含量降低,以至硬度和密度降低。这是由于在a-C:H:N薄膜中,并没有形成大量的比金刚石结构更硬的C_3N_4 (C≡N)相,主要形成了C-N键。因此,氮掺杂并不能使a-C:H薄膜满足硬盘要求。
在FCVA方法中,对70nm厚膜分析发现,当倾斜衬底角度增加时,ta-C薄膜中的sp~3含量降低,同时薄膜中的sp2团簇的振动更加有序,使得内应力将比硬度下降的更快。对2nm薄膜拉曼分析表明,当倾斜衬底增加时,其内应力和硬度也会下降。这是由于当衬底倾斜时,入射离子形成平行于衬底表面的动量,不仅降低薄膜的sp~3相的形成,而且促使sp2相更加有序。
在FCVA方法中,对衬底偏压的研究表明,与70nm厚膜偏压效应相反,首次发现对2nm薄膜来说,当衬底偏压增加时,sp~3含量几乎在线性降低,对应的硬度也降低。这是因为偏压可以诱导与衬底形成更多的混合键,这些混合键都比C-C键长,故降低了薄膜的硬度;而对于厚膜来讲,界面混合层的影响可以忽略不计,高能量入射离子导致较多的sp~3键的过程占主导作用。
对于磁头使用的多层材料,DLC薄膜在AlTiC上沉积时,sp~3含量最高,对应硬度最高;而在FeCo、FeNi上,薄膜中的sp~3含量较低;在Au上,sp~3含量最低。
最后,为有效评估DLC在纳米级Lead区域结合力建立了超声震荡加化学腐蚀的方法。发现薄膜在AuCu上的结合力强于Au。从而对于可能由于DLC/ Lead间弱的结合力而引起的磁阻材料氧化问题,本实验结果提供了一种方法,从Wafer设计层面上,通过AuCu取代Au作为lead材料加以研究解决。
With the development of magnetic disk drive technology, ultra-thin diamond-like carbon (DLC) films have attracted considerable interest as a protective overcoat. In this thesis, firstly, DLC films are deposited using electron cyclotron resonance (ECR) chemical vapor deposition、ion beam deposition optimization (IBO) and filtered cathodic vacuum arc (FCVA) techniques, respectively. Then we consider in detail the use of a combined study of Raman spectra taken at two wavelengths (514 and 244 nm) to study the structure of films that can reflect its properties, and this is highlight part of the thesis. In addition, we propose a method for ultra-thin DLC films adherence evaluation on the nano-scale lead area of magnetic recording slider. The details are as following:
Firstly DLC films of different thickness from 10? to 100? are prepared by ECR-CVD、IBO and FCVA techniques, respectively. Through Raman spectroscopy study, the growth model for three kinds of films was discussed. For a-C:H films by ECR-CVD and IBO, its formation process mainly includes two stages. When film thickness is less than 50?, the carbon ions will form multiple nucleation centers like island, and when thickness is over 50?, the films developed with layer model and its structure became stable. But for ta-C films by FCVA, its growth process includes three stages. At the first stage, the thickness is less than 15? and it developed with island-like model. At the second stage, the thickness is from 15? to 50?, it developed with layer-like model and it already became stable. For the third stage, the thickness is over 50?, in mass area it could be described by layer model, while in local area it is with island model to form a little more tetrahedral structure. Thus, ta-C films of thickness over 15 ? already became dense and continuous and it will be the best choice for application of films in magnetic recording slider.
By ECR-CVD with a mixed gas of CH4 and N_2, the structure and mechanical properties of the a-C:H:N films are studied. The results show that a-C:H:N films with higher N content will contain less sp~3 sites. Hardness test of films confirmed that more N content corresponds to lower hardness. It also indicates that hard C≡N bond with high energy state is difficult to be formed by plasma doping, and additional N can not improve mechanical properties for a-C:H.
The tetrahedral amorphous carbon (ta-C) films by FCVA have been studied as a function of oblique angles of substrates varied from 0 to 60o, while keeping the energy of incident particles stable. The films contain less sp~3 sites and more ordered sp2 clustering as the substrate tilting for thicker films of 70 nm, and also a decrease of sp~3 content of ultra-thin films of 2 nm. Also it was found that the tilting can dramatically lower internal stress with less influence on hardness because hardness is related to sp~3 content, while internal stress is not only related to sp~3 content but also related to the order of sp2 cluster.
Additionally, substrate bias effect on ta-C film is studied. We found that the sp~3 content of 70 nm films increases with higher bias, while sp~3 content of 2 nm ultra-thin films falls almost linearly with bias. This is because substrate bias enhances mixing between the carbon films and substrate, and these mixing bonds are longer than C-C bonds. But for thicker films, the effect of mixing layer can be negligible compared to bias with higher carbon ion energy.
The sliders are composed of multi-layers which are mainly Fe-Co (Fe: 67%at, Co: 33%at) alloy, Fe-Ni (Fe: 18%at, Ni: 82%at) alloy, Au and Al_2O_3-TiC (Al_2O_3: 64%at, TiC: 36%at). The spectra show that the films deposited on Al_2O_3-TiC contains the highest sp~3 content, less sp~3 content on Fe-Co and Fe-Ni alloy, and the lowest of sp~3 content on Au substrate. It also indicates that the sequence of the anti-wear performance of ta-C film on different substrates is Al_2O_3-TiC > Fe-Co and Fe-Ni alloy > Au.
Finally, we propose a method with ultra-sonic plus chemical etching test, for ultra-thin Si/DLC films adherence evaluation on the nano-scale lead area of magnetic recording slider. The adherences of films on both Au and Au-Cu (Au: 93%at, Cu: 7%at) based lead are compared, and the results show Au-Cu lead exhibits better adhesion to Si/DLC than that with Au as confirmed by nano-scratch tests from the wafer level.
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