多层介质膜脉宽压缩光栅清洗方法研究

doi:10.15541/jim20190054

无机材料学报 ›› 2019, Vol. 34 ›› Issue (12): 1285-1289.DOI: 10.15541/jim20190054 CSTR: 32189.14.10.15541/jim20190054

多层介质膜脉宽压缩光栅清洗方法研究

邹溪^1,^2,^3,⁴,晋云霞^1,²,孔钒宇^1,²,王勇禄^1,²,张益彬^1,²,邵建达^1,²()

^1. 中国科学院上海光学精密机械研究所, 薄膜光学实验室, 上海 201800
^2. 中国科学院强激光材料重点实验室, 上海 201800
^3. 中国科学院大学材料与光电研究中心, 北京 100049
^4. 上海科技大学物质科学与技术学院, 上海 201210

收稿日期:2019-01-28 修回日期:2019-03-08 出版日期:2019-12-20 网络出版日期:2019-05-29
作者简介:邹溪(1993-), 男, 硕士研究生. E-mail:zouxi@siom.ac.cn
基金资助:
国家自然科学基金重点项目(11604352);国家自然科学基金重点项目(61875212);上海市科学技术委员会(16JC1420600)

Cleaning Methods for Multilayer Dielectric Pulse Compression Gratings

ZOU Xi^1,^2,^3,⁴,JIN Yun-Xia^1,²,KONG Fan-Yu^1,²,WANG Yong-Lu^1,²,ZHANG Yi-Bin^1,²,SHAO Jian-Da^1,²()

^1. Laboratory of Thin Film Optics, Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800, China
^2. Key Laboratory of Materials for High Power Laser, Chinese Academy of Sciences, Shanghai 201800, China
^3. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
^4. School of Physical Science and Technology, Shanghai Tech University, Shanghai 201210, China

Received:2019-01-28 Revised:2019-03-08 Published:2019-12-20 Online:2019-05-29
Supported by:
National Natural Science Foundation of China(11604352);National Natural Science Foundation of China(61875212);Science and Technology Commission of Shanghai Municipality(16JC1420600)

摘要/Abstract

摘要：

采用SPM (Sulfuric-Peroxide Mixtures, 98wt%H₂SO₄+30wt%H₂O₂)+兆声(方法1)和氧等离子体+HPM (Hydrochloric/Peroxide Mixture, 37wt%HCl+30wt%H₂O₂+DIH₂O)+兆声(方法2)两种清洗方法对多层介质膜脉宽压缩光栅进行清洗, 并对清洗前后样品的表面元素含量、衍射效率、表面粗糙度、表面温升以及激光损伤阈值等参数进行测量以评估两种清洗方法清洗效果。在入射角70°, 脉宽12 ns, s偏振, 波长1064 nm的激光辐照下, 经过清洗方法1清洗后的光栅样品单脉冲激光损伤阈值为7.55 J/cm ², 而方法2清洗后的样品损伤阈值为5.32 J/cm ²。另外, 虽然经过方法2清洗后样品表面杂质含量更低, 但是在衍射效率、表面粗糙度和表面温升都劣于经方法1清洗后的样品, 进一步分析发现方法2中氧等离子体清洗过程引入的Fe元素影响了其样品损伤性能和温升性能。因此, SPM清洗方法可以作为多层介质膜脉宽压缩光栅提升抗激光损伤性能的优化清洗方案。

关键词: 多层介质膜, 脉宽压缩光栅, 氧等离子体, SPM, HPM

Abstract:

Two cleaning methods for multilayer dielectric pulse compression gratings (MDG) were studied. The first method is SPM (Sulfuric-Peroxide Mixtures, 98wt%H₂SO₄+30wt%H₂O₂) + megasonic, and the second method is Oxygen plasma + HPM (Hydrochloric/Peroxide Mixture, 37wt%HCl+30wt%H₂O₂+DIH₂O) + megasonic. To compare the cleaning effectiveness, the element content of sample surface, diffraction efficiency, surface roughness, temperature rising and laser damage induced threshold (LIDT) were measured. The 1-on-1 LIDT of samples cleaned by the first and the second methods are 7.55 and 5.32 J/cm ² respectively, with 1064 nm laser pulse (12 ns, s-polarized) at incidence angle of 70°. In addition, the sample cleaned by the second method has lower surface contamination content, but the sample cleaned by the first method has better performance in diffraction efficiency, surface roughness and temperature rising. By further analyzing, we find that element Fe brought by oxygen plasma cleaning process in the second method is the factor that affects the damage performance and temperature rising. Therefore, the cleaning method based on the first one, the SPM + megasonic is better for improving the laser damage performance of MDG.

Key words: multilayer dielectric, pulse compression grating, oxygen plasma, SPM, HPM

中图分类号:

TH745

邹溪, 晋云霞, 孔钒宇, 王勇禄, 张益彬, 邵建达. 多层介质膜脉宽压缩光栅清洗方法研究[J]. 无机材料学报, 2019, 34(12): 1285-1289.

ZOU Xi, JIN Yun-Xia, KONG Fan-Yu, WANG Yong-Lu, ZHANG Yi-Bin, SHAO Jian-Da. Cleaning Methods for Multilayer Dielectric Pulse Compression Gratings[J]. Journal of Inorganic Materials, 2019, 34(12): 1285-1289.

图/表 9

图1 多层介质膜脉宽压缩光栅的制备流程

Fig. 1 Fabrication process of multilayer dielectric pulse compression grating

图2 两种清洗方法的清洗流程

Fig. 2 Cleaning processes of two cleaning methods

图3 未清洗的样品和两种清洗方法清洗后样品的元素含量以及表面杂质(Surface Contaminants, SC)含量

Fig. 3 Element contents and surface contaminants (SC) contents of uncleaned sample and cleaned samples by two cleaning methods

图4 未清洗样品和两种清洗方法清洗后样品的-1级衍射效率

Fig. 4 The -1st diffraction efficiencies (DE) of uncleaned sample and cleaned samples by two cleaning methods

图5 原子力显微镜测试的未清洗样品和两种清洗方法清洗后样品的表面形貌

Fig. 5 Surface morphologies of uncleaned sample and cleaned samples by two cleaning methods measured by AFM

图6 未清洗样品和两种清洗方法清洗后样品表面温度随激光功率的变化

Fig. 6 Surface temperature of the uncleaned samples and cleaned samples by two cleaning methods changed with the laser power

图7 激光损伤测试系统

Fig. 7 The laser damage testing system

表1 两种方法清洗后样品的损伤阈值

Table 1 Laser damage threshold of samples cleaned by two cleaning methods

Cleaning method	SPM (method 1)	Oxygen plasma + HPM (method 2)
LIDT/(J?cm^-2)	7.55	5.32

表2 方法2单步清洗后Fe元素含量

Table 2 Content of Fe element after the single step in cleaning method

Cleaning process	Post-oxygen plasma	Post-HPM
Fe/at%	7.55	2.1

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多层介质膜脉宽压缩光栅清洗方法研究

Cleaning Methods for Multilayer Dielectric Pulse Compression Gratings

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