离子源偏压对PIA-EB-Hf法制备的HfO2激光薄膜性能的影响

doi:10.15541/jim20160170

摘要/Abstract

摘要：

探究HfO₂薄膜的激光损伤特性以进一步提高激光损伤阈值(Laser Induced Damage Threshold, 简称LIDT), 对其在高功率激光系统中的广泛应用具有重要的意义。在不同的离子源偏压下, 采用等离子体辅助电子束蒸发金属铪(Hf)并充氧(O₂)进行反应沉积法制备了中心波长为1064 nm, 光学厚度为4H的HfO₂薄膜样品。测试了薄膜组分和残余应力; 根据透射谱拟合了薄膜的折射率; 通过XRD谱图和SEM表面形貌图分析了薄膜的微观结构; 对激光损伤阈值、损伤特性和机理进行了论述。结果表明: 偏压100 V时制备的薄膜具有最佳O/Hf配比; 薄膜压应力和折射率均随偏压降低而减小。薄膜内存在结晶, 激光能量在晶界缺陷处被强烈聚集和吸收, 加速了膜层的破坏, 形成由几百纳米的烧灼坑聚集而成的海绵状损伤结构。随着偏压降低, 膜结晶取向由( $1 ? 11$ )晶面向(002)晶面转变, 界面能降低; 晶粒减小, 结构更均匀, 缓解了激光能量在晶界处的局部聚集与吸收, 表现出较大的激光损伤阈值。

关键词: HfO2薄膜, 等离子体辅助电子束蒸发, 离子源偏压, 微观结构, 激光损伤

Abstract:

The anti laser HfO₂films were deposited by reactive plasma ion assisted electron beam evaporation in low O₂-pressure with different Advanced Plasma Source (APS) bias voltages. Properties of HfO₂ film sincluding chemical composition, refractive index and residual stress were investigated. Microstructure of HfO₂films was analyzed by scanning electron microscope (SEM) and X-ray diffraction (XRD). Laser induced damage threshold (LIDT) and damage mechanisms of HfO₂ films were finally evaluated and discussed. Properties of HfO₂ films display sensitive to APS bias voltage. As the APS bias voltage decreases, the O/Hf ratio in the film increases, accompanied by decreasing refractive index and residual stress. The damage morphology of HfO₂ films appears in the form of agglomerations of craters with a few hundreds of nanometers, left by evaporation of grains ascribed to strong absorption and accumulation of laser energy at grain-boundaries. HfO₂ films with higher LIDT can be grown under lower bias voltage which benefits the achievement of uniform microstructure and the crystallization orientation from ( $1 ? 11$ ) plane to (002) plane with low grain boundary energy and lattice defects.

Key words: HfO2 film, plasma-assisted electron beam evaporation, bias voltage, microstructure, laser damage

中图分类号:

O484

付朝丽, 杨勇, 马云峰, 魏玉全, 焦正, 黄政仁. 离子源偏压对PIA-EB-Hf法制备的HfO₂激光薄膜性能的影响[J]. 无机材料学报, 2017, 32(1): 69-74.

FU Chao-Li, YANG Yong, MA Yun-Feng, WEI Yu-Quan, JIAO Zheng, HUANG Zheng-Ren. APS Bias Voltage on Properties of HfO₂ Laser Films Deposited by Reactive Plasma Ion Assisted Electron Evaporation[J]. Journal of Inorganic Materials, 2017, 32(1): 69-74.

图/表 10

表1 HfO2薄膜的沉积工艺

Table 1 Deposition conditions of HfO2 films

Samples	APS bias voltage/V	APS discharge current/A	Rate/(nm·s^-1)	Temperature/℃	EBG-O₂/sccm	APS-O₂/sccm
1#	120	55	0.1	200	30	45
2#	110	55	0.1	200	30	45
3#	100	55	0.1	200	30	45
4#	90	55	0.1	200	30	45
5#	70	55	0.1	200	30	45

图1 曲率半径计算原理图

Fig. 1 Schematic illustration of the curvature radius calculation

图2 HfO2薄膜的化学元素组成EDS图谱

Fig. 2 EDS pattern of the HfO2 film

图3 离子源偏压对HfO2薄膜O/Hf配比的影响

Fig. 3 Effect of APS bias voltage on the O/Hf ratio of HfO2 films

图4 不同离子源偏压下制备的HfO2薄膜的光学特性

Fig. 4 Optical properties of HfO2 films deposited at different APS bias voltages(a) Transmittance spectra; (b) Refractive index dispersion spectra

图5 离子源偏压对HfO2薄膜残余应力的影响

Fig. 5 Effect of APS bias voltage on the residual stress of HfO2 films

图6 不同离子源偏压下制备的HfO2薄膜的XRD图谱

Fig. 6 XRD patterns of HfO2 films deposited at different APS bias voltages

图7 不同离子源偏压下制备的HfO2薄膜的表面形貌

Fig. 7 SEM images of HfO2 films deposited at different bias voltages(a) 120 V; (b) 110 V; (c) 100 V; (d) 90 V

图8 不同离子源偏压下制备的HfO2薄膜的LIDT值测试结果

Fig. 8 LIDT of HfO2 films deposited at different APS bias voltages

图9 HfO2薄膜的激光损伤形貌和微观结构图

Fig. 9 SEM images of the laser damaged HfO2 film deposited at bias voltage of 90 VAt fluence of (a) 4.6 J/cm2; (b) 6 J/cm2; (c) 6 J/cm2

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离子源偏压对PIA-EB-Hf法制备的HfO₂激光薄膜性能的影响

APS Bias Voltage on Properties of HfO₂ Laser Films Deposited by Reactive Plasma Ion Assisted Electron Evaporation

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Samples	APS bias voltage/V	APS discharge current/A	Rate/(nm·s^-1)	Temperature/℃	EBG-O₂/sccm	APS-O₂/sccm
1#	120	55	0.1	200	30	45
2#	110	55	0.1	200	30	45
3#	100	55	0.1	200	30	45
4#	90	55	0.1	200	30	45
5#	70	55	0.1	200	30	45

Samples	APS bias voltage/V	APS discharge current/A	Rate/(nm·s^-1)	Temperature/℃	EBG-O₂/sccm	APS-O₂/sccm
1#	120	55	0.1	200	30	45
2#	110	55	0.1	200	30	45
3#	100	55	0.1	200	30	45
4#	90	55	0.1	200	30	45
5#	70	55	0.1	200	30	45

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Samples	APS bias voltage/V	APS discharge current/A	Rate/(nm·s^-1)	Temperature/℃	EBG-O₂/sccm	APS-O₂/sccm
1#	120	55	0.1	200	30	45
2#	110	55	0.1	200	30	45
3#	100	55	0.1	200	30	45
4#	90	55	0.1	200	30	45
5#	70	55	0.1	200	30	45

Samples	APS bias voltage/V	APS discharge current/A	Rate/(nm·s^-1)	Temperature/℃	EBG-O₂/sccm	APS-O₂/sccm
1#	120	55	0.1	200	30	45
2#	110	55	0.1	200	30	45
3#	100	55	0.1	200	30	45
4#	90	55	0.1	200	30	45
5#	70	55	0.1	200	30	45