退火温度对宽带脉冲压缩光栅载体金属/介质多层高反膜的影响

doi:10.15541/jim20140025

摘要/Abstract

摘要：

分别以金(Au)作为金属层材料, 氧化铪(HfO₂)与氧化硅(SiO₂)作为高低折射率层材料, 利用物理气相沉积方法制备了用于宽带脉冲压缩光栅制作的金属/介质多层高反膜, 研究了退火温度对其表面均方根粗糙度、反射率及抗化学清洗破坏能力的影响。实验结果表明: 退火前后样品表面均方根粗糙度变化很小; 提高退火温度能提高金属/介质多层膜的抗化学清洗破坏能力, 但反射率会随之下降。250℃退火10 h后金属/介质多层膜不仅可以承受住化学清洗过程, 而且反射率下降也比较小, 可以作为金属/介质多层膜的最佳退火工艺。

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关键词: 金属/介质多层膜, 脉冲压缩光栅, 退火, 化学清洗, 反射率

Abstract:

Metal/dielectric multilayers were prepared by physical vapor deposition process using gold as the metal material, HfO₂ and SiO₂ as high and low refractive index materials, respectively. These stacks were used to fabricate broadband pulse compression gratings. Influences of annealing temperature on the surface root-mean-square roughness, reflectivity and resistance to chemical cleaning damage were investigated. The experimental results indicated that surface root-mean-square roughness of these multilayers changed only slightly after annealing. Their resistance to chemical cleaning damage improved with the annealing temperature increase, whereas their reflectivity decreased. The metal/dielectric multilayers annealed at 250℃ for 10 h could not only endure the process of chemical cleaning, but also slightly decrease the reflectivity, suggesting that it is an optimal annealing process for metal/dielectric multilayers.

Key words: metal/dielectric multilayers, pulse compression gratings, annealing, chemical cleaning, reflectivity

中图分类号:

TG174

吴建波, 晋云霞, 关贺元, 孔钒宇, 刘文文, 刘世杰, 易葵. 退火温度对宽带脉冲压缩光栅载体金属/介质多层高反膜的影响[J]. 无机材料学报, 2014, 29(10): 1087-1092.

WU Jian-Bo, JIN Yun-Xia, GUAN He-Yuan, KONG Fan-Yu, LIU Wen-Wen, LIU Shi-Jie, YI Kui. Effect of Annealing Temperature on Metal/Dielectric Multilayers for Fabricating Broadband Pulse Compression Gratings[J]. Journal of Inorganic Materials, 2014, 29(10): 1087-1092.

图/表 11

图1 退火前金属/介质多层膜断面的SEM照片

Fig. 1 Cross section SEM image of the as-deposited metal/ dielectric multilayers

图2 退火前金属/介质多层膜的反射率

Fig. 2 Reflectivity of the as-deposited metal/dielectric multilayers

图3 不同温度退火后样品的AFM形貌

Fig. 3 AFM morphologies of samples annealed at different temperatures

图4 不同温度退火后金属/介质多层膜样品的反射率

Fig. 4 Reflectivity of metal/dielectric films after being annealed at different temperatures

表1 金在波长700~900 nm的光学常数

Table1 Optical constants of gold in the wavelength range of 700-900 nm

λ/nm	n	k
689	0.160	3.80
730	0.164	4.35
775	0.174	4.86
827	0.188	5.39
886	0.210	5.88
954	0.236	6.47

图5 理论计算的金属/介质多层膜反射率与过渡层中金填隙率的关系

Fig. 5 Theoretical arithmetic relationship between reflectively of metal/dielectric multilayers and interstitial rate of gold in the interfacial layers

图6 200℃退火样品经化学清洗后表面出现的裂纹

Fig. 6 Craze on surface of the sample after being annealed at 200℃ and chemical cleaning

图7 介质膜脱落后边缘的轮廓

Fig. 7 Profile of the edge after the dielectric film peeling off

图8 不同温度退火样品经化学清洗后典型的SEM照片

Fig. 8 Typical SEM images of samples after being annealed at different temperatures and chemical cleaning

图9 化学清洗后样品表面XPS全谱

Fig. 9 XPS survey spectra of samples after chemical cleaning

图10 表面起伏与附加应力分布示意图

Fig. 10 Schematic of relationship between additional stress distributing and surface undulation

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