SiNx Coatings Deposited by Reactive High Power Impulse Magnetron Sputtering: Process Parameters Influencing the Nitrogen Content.
SiNx Coatings Deposited by Reactive High Power Impulse Magnetron Sputtering: Process Parameters Influencing the Nitrogen Content.
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DOI：
10.1021/acsami.6b05830
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发表时间：
2016-07
影响因子：
9.5
通讯作者：
Susann Schmidt;T. Hänninen;Cecilia Goyenola;Jonas Wissting;J. Jensen;L. Hultman;N. Göbbels;M. Tobler;H. Högberg
中科院分区：
文献类型：
--
作者：
Susann Schmidt;T. Hänninen;Cecilia Goyenola;Jonas Wissting;J. Jensen;L. Hultman;N. Göbbels;M. Tobler;H. Högberg
反应性高功率脉冲磁控溅射 (rHiPIMS) 用于沉积生物医学应用的氮化硅 (SiNx) 涂层。 SiNx 生长和等离子体表征是在工业镀膜机中进行的，使用 Si 靶材和 N2 作为反应气体。研究了 0 至 0.3 之间不同的 N2-Ar 流量比、脉冲频率、目标功率设置和基底温度对放电和 SiNx 涂层的 N 含量的影响。等离子体离子质谱分析显示，在 N2-Ar 流量比 <0.16 的低放电脉冲初始部分，电离分子的信号随着脉冲结束时 N2-Ar 流量比和脉冲关闭时间的增加而上升。朗缪尔探针测量显示，非反应放电的电子温度为 2-3 eV，过渡模式放电的电子温度为 5.0-6.6 eV。分别通过 X 射线光电子能谱、X 射线反射率、X 射线衍射和纳米压痕对 SiNx 涂层的组成、化学键结构、密度和机械性能进行了表征。 SiNx 沉积过程和涂层性能主要受 N2-Ar 流量比的影响，从而受 SiNx 薄膜中 N 含量的影响，在较小程度上受 HiPIMS 频率和功率设置以及基板温度的影响。增加 N2-Ar 流量比会导致生长速率降低，而 N 含量、涂层密度、残余应力和硬度则增加。 rHiPIMS 期间存在的前体物质的密度泛函理论计算证实了这些实验结果。
Reactive high power impulse magnetron sputtering (rHiPIMS) was used to deposit silicon nitride (SiNx) coatings for biomedical applications. The SiNx growth and plasma characterization were conducted in an industrial coater, using Si targets and N2 as reactive gas. The effects of different N2-to-Ar flow ratios between 0 and 0.3, pulse frequencies, target power settings, and substrate temperatures on the discharge and the N content of SiNx coatings were investigated. Plasma ion mass spectrometry shows high amounts of ionized isotopes during the initial part of the pulse for discharges with low N2-to-Ar flow ratios of <0.16, while signals from ionized molecules rise with the N2-to-Ar flow ratio at the pulse end and during pulse-off times. Langmuir probe measurements show electron temperatures of 2-3 eV for nonreactive discharges and 5.0-6.6 eV for discharges in transition mode. The SiNx coatings were characterized with respect to their composition, chemical bond structure, density, and mechanical properties by X-ray photoelectron spectroscopy, X-ray reflectivity, X-ray diffraction, and nanoindentation, respectively. The SiNx deposition processes and coating properties are mainly influenced by the N2-to-Ar flow ratio and thus by the N content in the SiNx films and to a lower extent by the HiPIMS frequencies and power settings as well as substrate temperatures. Increasing N2-to-Ar flow ratios lead to decreasing growth rates, while the N content, coating densities, residual stresses, and the hardness increase. These experimental findings were corroborated by density functional theory calculations of precursor species present during rHiPIMS.