高等学校化学学报

高等学校化学学报

• 研究论文 • 上一篇    下一篇

纳米空气柱阵列-SiO2复合超材料的制备和折射率调控

刘旭1,2，黄玉铸1，刘奇1，曹鸿涛1,2   

  1. 1. 中国科学院宁波材料技术与工程研究所 2. 中国科学院大学材料科学和光电子研究中心
  • 收稿日期:2025-11-05 修回日期:2025-12-28 网络首发:2025-12-29 发布日期:2025-12-29
  • 通讯作者: 曹鸿涛 E-mail:h_cao@nimte.ac.cn
  • 基金资助:
    浙江省尖兵科技计划项目(批准号: 2024C01243(SD2))和宁波市自然科学基金(批准号: 2021J201)资助

Fabrication and Refractive Index Tuning of Air Nanocolumn Array-Silica Composite Metamaterials

LIU Xu1,2, HUANG Yuzhu1, LIU Qi1, CAO Hongtao1,2   

  1. 1. Ningbo Institute of Materials Technology & Engineering, Chinese Academy of Sciences 2. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences
  • Received:2025-11-05 Revised:2025-12-28 Online First:2025-12-29 Published:2025-12-29
  • Supported by:
    Supported by the "Pioneer" and "Leading Goose" R&D Program of Zhejiang Province, China(No.2024C01243(SD2)) and the Natural Science Foundation of Ningbo City, China(No. 2021J201)

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摘要： 本文提出并验证了一种基于二次化学刻蚀宽范围调控折射率并获得超低折射率的新策略。首先，采用多靶磁控共溅射技术制备Ag纳米线阵列-SiO2复合超材料薄膜，经过一次化学刻蚀工艺后去除金属相从而成功构建出纳米空气柱阵列-SiO2复合超材料薄膜。但因其孔隙率有限，所以不能满足更低折射率之要求，为了解决这个问题，本文创新性地引入二次化学刻蚀实现对纳米空气柱阵列直径的扩孔来增大孔隙率，获得了具有超低折射率(<1.2)的超材料薄膜。利用光谱型椭偏仪和扫描电子显微镜对薄膜光学性能与微观结构进行表征，并基于各向异性有效介质理论(EMA)模型对椭偏参数Ψ和Δ进行拟合，得出孔隙率与各向异性折射率的对应关系，明确了一次刻蚀可实现的最低折射率水平。系统研究和总结出二次刻蚀时间与刻蚀液浓度对折射率变化的影响规律。本文提出的超低折射率调控方法具有良好的工艺可重复性，实现了寻常折射率在1.367-1.159之间、异常折射率在1.392-1.191宽范围内的可控制备。本研究为超低折射率材料的可控制备提供了新途径，在车载镜头、显示面板等光子器件中具备重要应用前景。

关键词: 超材料薄膜, 低折射率, 纳米空气柱阵列, 化学刻蚀, 磁控溅射

Abstract: This study proposes and validates a novel strategy for fabricating ultra-low refractive index films based on nanostructure regulation via secondary chemical etching. Initially, Ag nanowire array-silica composite metamaterial films were prepared using multi-target magnetron co-sputtering technology. After the first-step chemical etching process to remove the metallic phase, an air-nanocolumn array-silica composite metamaterial film was successfully constructed. However, due to the limited porosity achieved by the first etching step, the resulting refractive index could not meet the requirement for further reduction. To address this issue, this work innovatively introduces a secondary chemical etching step to enlarge the diameter of the air nanocolumns, thereby increasing the porosity and successfully obtaining a composite metamaterial with an ultra-low refractive index (<1.2). The optical properties and microstructure of the films were characterized using spectroscopic ellipsometry and scanning electron microscopy. Based on the anisotropic effective medium approximation (EMA) model, the ellipsometric parameters Ψ and Δ were fitted to establish the relationship between porosity and anisotropic refractive indices, clarifying the minimum refractive index achievable by the first etching step. The effects of secondary etching time and etchant concentration on the refractive index were systematically investigated, demonstrating that the proposed ultra-low refractive index tuning method exhibits excellent process repeatability. This enables the controllable preparation of films with an ordinary refractive index ranging from 1.367 to 1.159 and an extraordinary refractive index between 1.392 and 1.191. This research provides a new pathway for the controllable preparation of ultra-low refractive index materials, holding significant application potential in photonic devices such as automotive lenses and display panels.

Key words: Metamaterial film, Low refractive index, Nano-air column array, Chemical etching, Magnetron sputtering

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