氟化镁基底上HfO2中间层对Al2O3薄膜微观组织和力学性能的影响

doi:10.15541/jim20160030

摘要/Abstract

摘要：

采用电子束蒸镀技术在氟化镁基底上制备了单层Al₂O₃薄膜和含有HfO₂中间层的HfO₂/Al₂O₃双层薄膜。在空气中对所制备的薄膜进行1 h 600℃的退火处理。通过掠入角X射线衍射仪(GIXRD)、场发射扫描电镜(FE-SEM)、傅里叶变换红外光谱仪(FTIR)、纳米压痕和划痕法对薄膜的微观结构、红外透过率和力学性能进行了表征。结果表明: 退火处理后HfO₂/Al₂O₃双层薄膜中形成了一层树枝状的新层, 这种新层的硬度大于17.5 GPa。这种高硬度的新层能够保护氟化镁基底不被划伤。从GIXRD图谱中只能找到单斜相HfO₂的衍射峰, 而Al₂O₃薄膜仍然保持非晶态。从这些结果中可以推断出HfO₂从非晶态向单斜相的转变促进了这种树枝状新层的产生, 也正是这种新层提高了保护薄膜的力学性能。

关键词: HfO2中间层, Al2O3薄膜, 微观组织, 力学性能, 氟化镁基底

Abstract:

Al₂O₃ thin films with or without HfO₂ interlayer between Al₂O₃ and substrate were deposited on MgF₂ substrates by electron-beam evaporation technique. The as-deposited thin films were then annealed at 600℃ for 1 h to promote crystallization. The microstructure, IR transmittance and mechanical properties of the as-deposited and annealed samples were investigated by field emission scanning electron microscopy (FE-SEM), grazing incidence X-ray diffraction (GIXRD), Fourier Transform Infrared (FTIR) spectrometer, nanoindentation, and scratch tests, respectively. FE-SEM results show that a new branch-like layer is generated in annealed HfO₂/Al₂O₃double-layer thin films. The hardness of the newly formed layer is considered to be larger than 17.5 GPa. Because of the high hardness of the new layer, the MgF₂substrate can be protected from being drown out during scratch test. From GIXRD patterns, Al₂O₃ still remains amorphous while HfO₂ interlayer transforms from amorphous to monoclinic phase after annealing process. It could be deduced that it is the phase transformation of HfO₂ interlayer that promotes the formation of the harder branch-like layer.

Key words: HfO2 interlayer, Al2O3 thin film, microstructure, mechanical properties, MgF2 substrate

中图分类号:

TQ174

宋博, 赵丽丽, 陈笑迎, 游丽君, 宋力昕. 氟化镁基底上HfO₂中间层对Al₂O₃薄膜微观组织和力学性能的影响[J]. 无机材料学报, 2016, 31(7): 779-784.

SONG Bo, ZHAO Li-Li, CHEN Xiao-Ying, YOU Li-Jun, SONG Li-Xin. Effects of HfO₂ Interlayer on Microstructure and Mechanical Property of Al₂O₃ Thin Film on MgF₂ Substrate[J]. Journal of Inorganic Materials, 2016, 31(7): 779-784.

图/表 5

Fig. 1 GIXRD patterns of the as-deposited and annealed samples

Fig. 2 Cross-sectional FE-SEM images of the as-deposited and annealed samples (a) A1; (b) A2; (c) AH1; (d) AH2

Fig. 3 IR transmittance spectra of the uncoated MgF2, as-deposited and annealed samples in the range of 3-5 μm

Fig. 4 Mechanical properties obtained from nanoindentation tests (a) Elastic modulus as a function of penetration depth for as-deposited and annealed samples; (b) Hardness as a function of penetration depth for the same samples

Fig. 5 SEM images of scratch tracks of the as-deposited and annealed samples.(a) A1; (b) A2; (c)AH1; (d) AH2; (e) Higher resolution image of the selected area in Fig. 5(d)

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氟化镁基底上HfO₂中间层对Al₂O₃薄膜微观组织和力学性能的影响

Effects of HfO₂ Interlayer on Microstructure and Mechanical Property of Al₂O₃ Thin Film on MgF₂ Substrate

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