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无机材料学报

• 研究论文 •    

用于氟化钙超精密加工的二氧化铈抛光液的制备与性能研究

贾文卿1,2, 张政豪3, 汪俊4, 王梦霞4, 张传奇1,2, 姜大朋2,5, 张玲1,2, 寇华敏2,5, 王文中1,2,3   

  1. 1.中国科学院 上海硅酸盐研究所,关键陶瓷材料全国重点实验室,上海 200050;
    2.中国科学院大学 材料科学与光电工程中心,北京 100049;
    3.国科大杭州高等研究院 化学与材料科学学院,杭州 310024;
    4.中国科学院 上海光学精密机械研究所,上海 2018001;
    5.中国科学院 上海硅酸盐研究所,功能晶体与器件全国重点实验室,上海 201899
  • 收稿日期:2026-01-21 修回日期:2026-03-19
  • 通讯作者: 王文中, 研究员. E-mail: wzwang@mail.sic.ac.cn; 寇华敏,正高级工程师. E-mail: huaminkou@mail.sic.ac.cn
  • 作者简介:贾文卿(2000-), 男, 硕士研究生. E-mail: jiawenqing23@mails.ucas.ac.cn
  • 基金资助:
    国家自然科学基金(52172256, 52372248, 52450255); 上海市科委“探索者”项目(25TS1416100)

Preparation and Performance of Ceria-Based Slurry for Ultra-Precision Polishing of Calcium Fluoride

JIA Wenqing1,2, ZHANG Zhenghao3, WANG Jun4, WANG Mengxia4, ZHANG Chuanqi1,2, JIANG Dapeng2,5, ZHANG Ling1,2, KOU Huamin2,5, WANG Wenzhong1,2,3   

  1. 1. State Key Laboratory of High Performance Ceramics, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China;
    2. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China;
    3. School of Chemistry and Materials Science, Hangzhou Institute for Advanced Study, University of Chinese Academy of Sciences, Hangzhou 310024, China;
    4. Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800, China;
    5. State Key Laboratory of Functional Crystals and Device, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China
  • Received:2026-01-21 Revised:2026-03-19
  • Contact: WANG Wenzhong, professor. E-mail: wzwang@mail.sic.ac.cn; KOU Huamin, professor. E-mail: huaminkou@mail.sic.ac.cn
  • About author:JIA Wenqing (2000-), male, Master candidate. E-mail: jiawenqing23@mails.ucas.ac.cn
  • Supported by:
    National Natural Science Foundation of China (52172256, 52372248,52450255); Shanghai Municipal Science and Technology Commission "Explorer" Project (25TS1416100)

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摘要： 随着集成电路制程节点不断微缩,光刻系统对氟化钙(CaF2)光学材料的表面质量提出了原子级光滑度的苛刻要求。针对传统碱性二氧化硅抛光液去除速率低、易腐蚀等问题,本研究开发了一种用于氟化钙化学机械抛光的高效、稳定且环境友好的近中性二氧化铈(CeO2)抛光液。采用尿素沉淀法合成了三种不同粒径的单分散球形CeO2磨料,并以聚丙烯酸钠(PAAS)为分散剂、脂肪醇聚氧乙烯醚(AEO-9)为表面活性剂配制抛光液。系统研究了煅烧温度、磨料粒径及添加剂含量对抛光性能的影响,研究结果表明在500 ℃煅烧的CeO2磨料,添加0.2% PAAS和0.2% AEO-9(质量分数)条件下对CaF2的抛光性能最佳。其中,粒径140 nm的磨料可实现109 nm/min的材料去除速率,抛光后表面粗糙度(Ra)为0.12 nm;而粒径110 nm的磨料可获得Ra低至0.09 nm的超光滑表面,两者均优于传统碱性二氧化硅抛光液。激光损伤阈值测试表明,经优化抛光液处理的CaF2损伤阈值达6.4 J/cm2,相比二氧化硅抛光液(4.9 J/cm2)损伤阈值显著提升。电子顺磁共振光谱(EPR)和傅里叶变换红外光谱(FT-IR)分析证实,CeO2表面的Ce3+是提升化学活性的关键。接触角测试表明,PAAS和AEO-9可显著降低接触角,明显改善抛光液在CaF₂表面的润湿性。本研究为氟化钙的超精密加工提供了一种高效、环境友好的新策略。

关键词: 氟化钙, 化学机械抛光, 球形二氧化铈, 抛光液, 超精密加工

Abstract: The continuous downscaling of integrated circuit nodes demands atomic-level smoothness for calcium fluoride (CaF2) optical materials used in lithography systems. To overcome the limitations of conventional alkaline silica polishing slurries, namely low material removal rate (MRR) and corrosion issues, this study developed a high-efficiency, stable, and eco-friendly near-neutral ceria (CeO2) slurry for chemical mechanical polishing (CMP) of CaF2. Monodispersed spherical CeO2 abrasives with three particle sizes were synthesized via urea precipitation. Polishing slurries were prepared using sodium polyacrylate (PAAS) as dispersant and primary alcobol ethoxylate (AEO-9) as surfactant. Effects of calcination temperature, abrasive size, and additive content on polishing performance were systematically investigated. Optimal performance was achieved with CeO2 calcined at 500 ℃, 0.2% PAAS and 0.2% AEO-9 (in mass). Specifically, the slurry containing 140 nm abrasives delivered a MRR of 109 nm/min and a surface roughness after polishing (Ra) of 0.12 nm, while the slurry with 110 nm abrasives produced an ultra-smooth surface with an Ra as low as 0.09 nm, outperforming the traditional alkaline silica slurry. Laser-induced damage threshold tests revealed that CaF2 polished with the optimized slurry reached 6.4 J/cm2, significantly higher than the 4.9 J/cm2 obtained with the silica slurry. Electron paramagnetic resonance (EPR) and Fourier-transform infrared (FT-IR) spectroscopic analyses confirmed that Ce3+ species on the CeO2 surface is critical for enhancing chemical reactivity. The contact angle measurements with reduced contact angle showed PAAS and AEO-9 notably improved wettability. This study provides an efficient, eco-friendly strategy for ultraprecision machining of CaF2.

Key words: calcium fluoride, chemical mechanical polishing, spherical ceria, slurry, ultra-precision machining

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