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目的:优化钼表面直流磁控溅射镀镍薄膜的工艺,提出后续热处理方法。方法设计正交实验,探究溅射功率、溅射气压、负偏压和沉积时间对镍薄膜沉积速率和附着力的影响,从而优化工艺参数。利用扫描电镜和平整度仪对最佳工艺参数下制备的薄膜的组织结构进行表征,并研究后续热处理对薄膜附着力的影响。结果工艺参数对镀镍薄膜沉积速率影响的主次顺序为:功率>溅射气压>负偏压;对薄膜附着力的影响主次顺序为:负偏压>沉积时间>功率>溅射气压。随溅射功率增大,沉积速率增大,薄膜附着力先增后减;随溅射气压增大,沉积速率和薄膜附着力均先增后减。负偏压增大对沉积速率影响较小,但有利于提高薄膜附着力。随沉积时间延长,薄膜附着力降低。在氢气气氛下进行850℃×1 h的后续热处理,能够促进扩散层的形成,明显提高镍薄膜的附着力。结论最佳镀镍工艺参数为:溅射功率1.8 kW,溅射气压0.3 Pa,负偏压450 V,沉积时间10 min。在该条件下制备的镍薄膜厚度达到1.15μm左右,与基体结合紧密,表面平整、连续、致密。后续增加热处理工序是提高镍薄膜附着力的有效方法。

Objective To optimize the process of plating nickel film on molybdenum disc substrates by direct current magnetron sputtering, and research the follow-up heat treatment. Methods Though designing an orthogonal experiment scheme, the effects of sputtering power, sputtering pressure, bias voltage and deposition time on deposition rate and adhesion of nickel film were re-searched. The organization and structure of nickel film prepared with the optimal parameters were characterized by scanning elec-tron microscope and flatness tester. And the effect of follow-up heat treatment on adhesion of nickel film was also researched. Results The results showed that the primary and secondary order of the effects of the parameters on the deposition rate was:sputte-ring power, sputtering pressure and then bias voltage. The primary and secondary order of the effects of the parameters on the adhe-sion was:bias voltage, deposition rate, sputtering power, and then sputtering pressure. With increasing sputtering power, the dep-osition rate increased and the film adhesion increased at first and then decreased. With increasing deposition time, the deposition rate and film adhesion both increased at first and then decreased. Negative bias had little effect on the deposition rate, but it was beneficial for improving the adhesion of the film. And the film adhesion decreased with the increase of deposition time. The follow-up heat treatment of 1 h incubation at 850 ℃ in hydrogen atmosphere could obviously increase the film adhesion by promoting the formation of the diffusion layer. Conclusion The optimal process parameters of plating nickel film were:sputtering power 1. 8 kW, sputtering pressure 0. 3 Pa, bias voltage 450 V,deposition time 10 min. The thickness of th film was about 1. 15μm. The film and substrate bounded tightly, and the surface of film was smooth, continuous and dense. The follow-up heat treatment was an effective method to improve the adhesion of nickel film.

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