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

doi:10.15541/jim20260041

无机材料学报 ›› 2026, Vol. 41 ›› Issue (10): 1425-1434.DOI: 10.15541/jim20260041

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 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 201800
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 出版日期:2026-10-20 网络出版日期:2026-04-03
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);国家自然科学基金(52372248);国家自然科学基金(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 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 Published:2026-10-20 Online:2026-04-03
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);National Natural Science Foundation of China(52372248);National Natural Science Foundation of China(52450255);Shanghai Municipal Science and Technology Commission “Explorer” Project(25TS1416100)

摘要/Abstract

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CaF₂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, 以500 ℃煅烧的CeO₂为磨料, 添加0.2% PAAS和0.2% AEO-9 (质量分数)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(R_a)为0.12 nm; 而粒径110 nm的磨料可获得R_a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, 经优化的CeO₂抛光液处理的CaF₂损伤阈值达6.4 J/cm², 较二氧化硅抛光液(4.9 J/cm²)提升了约31%。电子顺磁共振(EPR)光谱和傅里叶变换红外(FT-IR)光谱分析证实, 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CaF₂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, then the polishing slurries were prepared using sodium polyacrylate (PAAS) as dispersant and primary alcohol 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 ℃ in the presence of 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 (R_a) of 0.12 nm, while the slurry with 110 nm abrasives produced an ultra-smooth surface with an R_a 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, which is approximately 31% 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 are critical for enhancing chemical reactivity. The contact angle measurements showed that PAAS and AEO-9 notably reduced contact angle and 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

中图分类号:

TN305

贾文卿, 张政豪, 汪俊, 王梦霞, 张传奇, 姜大朋, 张玲, 寇华敏, 王文中. 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[J]. 无机材料学报, 2026, 41(10): 1425-1434.

JIA Wenqing, ZHANG Zhenghao, WANG Jun, WANG Mengxia, ZHANG Chuanqi, JIANG Dapeng, ZHANG Ling, KOU Huamin, WANG Wenzhong. Preparation and Performance of Ceria-based Slurry for Ultra-precision Polishing of Calcium Fluoride[J]. Journal of Inorganic Materials, 2026, 41(10): 1425-1434.

图/表 19

表1 氟化钙抛光参数

Table 1 Polishing parameters of CaF2

Parameter	Condition
Pressure/kPa	4.0
Polishing controller speed/(r·min^-1)	15
Polishing pad speed/(r·min^-1)	60
Slurry flow rate/(mL·min^-1)	8.0
Polishing time/min	20

表2 接触角测试的抛光液的组成

Table 2 Composition of slurry for contact angle testing

Slurry	Composition (mass fraction)
S1	2% CeO₂
S2	2% CeO₂+ 0.2% PAAS
S3	2% CeO₂+ 0.2% PAAS + 0.1% AEO-9
S4	2% CeO₂+ 0.2% PAAS + 0.2% AEO-9
S5	2% CeO₂+ 0.2% PAAS + 0.5% AEO-9
S6	2% CeO₂+ 0.2% PAAS + 1% AEO-9

图1 二氧化铈的SEM照片和粒径分布

Fig. 1 SEM images and particle size distributions of ceria (a, d) CeO2-1; (b, e) CeO2-2; (c, f) CeO2-3

图2 不同温度煅烧后二氧化铈的XRD图谱

Fig. 2 XRD patterns of ceria calcined at different temperatures

图3 抛光液的Zeta电位随(a) PAAS含量及(b) AEO-9含量(添加0.5% PAAS)的变化

Fig. 3 Zeta potential variation with (a) PAAS and (b) AEO-9 contents (with addition of 0.5% PAAS) of the polishing slurry

图4 不同温度煅烧的CeO2-2作为磨料, MRR随抛光液中成分含量的变化

Fig. 4 Variation of MRR with slurry composition using CeO2-2 calcined at different temperatures as abrasive (a) Variation with PAAS content; (b) Variation with AEO-9 content with addition of 0.2% PAAS

图5 氟化钙抛光后表面的金相显微镜照片

Fig. 5 Metallographic microscope images of polished calcium fluoride surfaces (a) After coarse polishing; (b) CeO2; (c) CeO2 + 0.2% PAAS; (d) CeO2 + 0.2% PAAS + 0.1% AEO-9; (e) CeO2 + 0.2% PAAS + 0.2% AEO-9; (f) CeO2 + 0.2% PAAS + 0.5% AEO-9

图6 不同抛光液抛光后CaF2表面的三维形貌

Fig. 6 3D morphologies of CaF2 surfaces polished with different slurries (a) CeO2-1 + 0.2% PAAS + 0.2% AEO-9; (b) CeO2-2 + 0.2% PAAS + 0.2% AEO-9; (c) SiO2 + 0.2% PAAS + 0.2% AEO-9, pH 11; (d) FUJIMI Compol-80 slurry. Colorful figures are available on website

图7 (a)自制碱性SiO2抛光液和(b) CeO2-2抛光液双面抛光后氟化钙的激光损伤曲线

Fig. 7 Laser damage curves of calcium fluoride after double-sided polishing with (a) self-made alkaline SiO2 polishing slurry and (b) CeO2-2 polishing slurry

图8 不同条件处理的CeO2的EPR谱图及其局部放大图

Fig. 8 EPR spectra of CeO2 treated under different conditions and their magnified views (a, b) CeO2-2 calcined at different temperatures; (c, d) CeO2 with different particle sizes calcined at 500 ℃

图9 不同温度煅烧的CeO2-2抛光前后的FT-IR谱图

Fig. 9 FT-IR spectra of CeO2-2 (calcined at different temperatures) before and after polishing

图10 不同抛光液在CaF2表面的接触角

Fig. 10 Contact angles of different slurries on CaF2 surface

图S1 不同PAAS含量抛光液的稳定性随保存天数的变化

Fig. S1 Stability of polishing slurries with different PAAS contents over storage time (PAAS addition from left to right: 0, 0.1%, 0.2%, 0.5%, 1%)

表S1 以CeO2粒径、PAAS含量及AEO-9含量为变量的正交实验结果

Table S1 Results of orthogonal experiments with CeO2 particle size, PAAS content, and AEO-9 content as variables

Number	Size of CeO₂/nm	PAAS/% (in mass)	AEO-9/% (in mass)	MRR/(nm·min^-1)	Surface quality
1	110	0	0	71	1
2	110	0.1	0.1	96	3
3	110	0.2	0.2	99	5
4	110	0.5	0.5	79	2
5	110	1	1	70	2
6	110	0	0.1	74	2
7	110	0.1	0.2	100	4
8	110	0.2	0.5	89	2
9	110	0.5	1	66	2
10	110	1	0	120	3
11	140	0	0.2	67	1
12	140	0.1	0.5	80	2
13	140	0.2	1	67	2
14	140	0.5	0	129	3
15	140	1	0.1	120	3
16	140	0	0.5	56	1
17	140	0.1	1	60	1
18	140	0.2	0	120	3
19	140	0.5	0.1	122	4
20	140	1	0.2	115	5
21	210	0	1	38	1
22	210	0.1	0	95	2
23	210	0.2	0.1	109	3
24	210	0	0.2	97	5
25	210	1	0.5	89	2

图S2 500 ℃煅烧的不同粒径二氧化铈的MRR

Fig. S2 MRR of ceria with different particle sizes calcined at 500 ℃

图S3 不同粒径的二氧化铈及在不同温度煅烧的二氧化铈抛光后的表面

Fig. S3 Polished surfaces of ceria with different particle sizes and calcination temperatures (a) CeO2-1, (b) CeO2-3 calcined at 500 ℃; CeO2-2 calcined at (c) 400 ℃, (d) 600 ℃

图S4 实验室自制二氧化硅的(a) SEM照片和(b)粒径分布

Fig. S4 (a) SEM image and (b) particle size distribution of the lab-synthesized silica

图S5 不同抛光液的MRR

Fig. S5 MRR of different polishing slurries

表S2 其他研究工作氟化钙抛光参数及性能与本研究工作的比较

Table S2 Comparison of the polishing parameters and performance of calcium fluoride between existing studies and this work

Polished object	Polishing method	Polishing slurry composition	Polishing parameters	Optimal polishing result	Reference
CaF₂	CMP	SiO₂, KOH, pH 9.5-10	Pressure: 44 kPa, Speed: 120 r/min	R_q=0.37 nm	[S1]
CaF₂	CMP	50 nm SiO₂, pH 11		R_q=0.18 nm	[S2]
CaF₂	CMP	SiO₂, alkaline conditions		R_a=0.68 nm	[S3]
CaF₂	Magnetorheological polishing (MRP)	6% diamond abrasive	Speed: 500 r/min, Excitation Gap:10 mm	R_a=0.03 μm	[S4]
CaF₂	MRP + Ion beam polishing (IBP)	MRP: CeO₂+ surfactant + Fe(OH)₃; IBP: Ar⁺ beam	MRP speed: 550 r/min; IBP: 400 eV	MRR: MRP=1.33 μm/min, IBP=3 nm/min, R_a=1.44 nm	[S5]
CaF₂	Single point diamond turning (SPDT)		Speed: 3000 r/min	R_a=2.84 nm	[S6]
CaF₂	Float polishing (FP)	3% 7 nm SiO₂	Speed: 78 r/min	R_q=0.08 nm	[S7]
CaF₂	CMP	2% CeO₂+ 0.2% PAAS + 0.2% AEO-9	Pressure: 7.8 kPa; Speed: 60 r/min	MRR=99 nm/min, R_a=0.09 nm	This work

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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

Preparation and Performance of Ceria-based Slurry for Ultra-precision Polishing of Calcium Fluoride

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Number	Size of CeO₂/nm	PAAS/% (in mass)	AEO-9/% (in mass)	MRR/(nm·min^-1)	Surface quality
1	110	0	0	71	1
2	110	0.1	0.1	96	3
3	110	0.2	0.2	99	5
4	110	0.5	0.5	79	2
5	110	1	1	70	2
6	110	0	0.1	74	2
7	110	0.1	0.2	100	4
8	110	0.2	0.5	89	2
9	110	0.5	1	66	2
10	110	1	0	120	3
11	140	0	0.2	67	1
12	140	0.1	0.5	80	2
13	140	0.2	1	67	2
14	140	0.5	0	129	3
15	140	1	0.1	120	3
16	140	0	0.5	56	1
17	140	0.1	1	60	1
18	140	0.2	0	120	3
19	140	0.5	0.1	122	4
20	140	1	0.2	115	5
21	210	0	1	38	1
22	210	0.1	0	95	2
23	210	0.2	0.1	109	3
24	210	0	0.2	97	5
25	210	1	0.5	89	2

Number	Size of CeO₂/nm	PAAS/% (in mass)	AEO-9/% (in mass)	MRR/(nm·min^-1)	Surface quality
1	110	0	0	71	1
2	110	0.1	0.1	96	3
3	110	0.2	0.2	99	5
4	110	0.5	0.5	79	2
5	110	1	1	70	2
6	110	0	0.1	74	2
7	110	0.1	0.2	100	4
8	110	0.2	0.5	89	2
9	110	0.5	1	66	2
10	110	1	0	120	3
11	140	0	0.2	67	1
12	140	0.1	0.5	80	2
13	140	0.2	1	67	2
14	140	0.5	0	129	3
15	140	1	0.1	120	3
16	140	0	0.5	56	1
17	140	0.1	1	60	1
18	140	0.2	0	120	3
19	140	0.5	0.1	122	4
20	140	1	0.2	115	5
21	210	0	1	38	1
22	210	0.1	0	95	2
23	210	0.2	0.1	109	3
24	210	0	0.2	97	5
25	210	1	0.5	89	2

[1]	王华进, 寇华敏, 王墉哲, 姜大朋, 张博, 钱小波, 王静雅, 朱琳玲, 曾爱军, 杨秋红, 苏良碧. 193 nm激光下不同含量Y杂质CaF₂晶体辐照损伤研究[J]. 无机材料学报, 2023, 38(2): 219-224.
[2]	汪为磊, 刘卫丽, 白林森, 宋志棠, 霍军朝. 氧化铝颗粒的表面改性及其在C平面(0001)蓝宝石衬底上的化学机械抛光(CMP)性质[J]. 无机材料学报, 2017, 32(10): 1109-1114.
[3]	王宝基,张兴堂,薛中会,戴树玺,李蕴才,黄亚彬,杜祖亮. 利用Langmuir单层膜诱导合成CaF₂单晶[J]. 无机材料学报, 2006, 21(1): 12-16.
[4]	蔡舒,王彦伟,李金有,关勇辉,姚康德. 分散介质和矿化剂CaF₂对合成α-磷酸钙的影响[J]. 无机材料学报, 2004, 19(4): 852-858.
[5]	董永军,周国清,杨卫桥,苏良碧,徐军. 光刻系统用氟化钙晶体的研究进展[J]. 无机材料学报, 2004, 19(3): 449-455.

Number	Size of CeO₂/nm	PAAS/% (in mass)	AEO-9/% (in mass)	MRR/(nm·min^-1)	Surface quality
1	110	0	0	71	1
2	110	0.1	0.1	96	3
3	110	0.2	0.2	99	5
4	110	0.5	0.5	79	2
5	110	1	1	70	2
6	110	0	0.1	74	2
7	110	0.1	0.2	100	4
8	110	0.2	0.5	89	2
9	110	0.5	1	66	2
10	110	1	0	120	3
11	140	0	0.2	67	1
12	140	0.1	0.5	80	2
13	140	0.2	1	67	2
14	140	0.5	0	129	3
15	140	1	0.1	120	3
16	140	0	0.5	56	1
17	140	0.1	1	60	1
18	140	0.2	0	120	3
19	140	0.5	0.1	122	4
20	140	1	0.2	115	5
21	210	0	1	38	1
22	210	0.1	0	95	2
23	210	0.2	0.1	109	3
24	210	0	0.2	97	5
25	210	1	0.5	89	2

Number	Size of CeO₂/nm	PAAS/% (in mass)	AEO-9/% (in mass)	MRR/(nm·min^-1)	Surface quality
1	110	0	0	71	1
2	110	0.1	0.1	96	3
3	110	0.2	0.2	99	5
4	110	0.5	0.5	79	2
5	110	1	1	70	2
6	110	0	0.1	74	2
7	110	0.1	0.2	100	4
8	110	0.2	0.5	89	2
9	110	0.5	1	66	2
10	110	1	0	120	3
11	140	0	0.2	67	1
12	140	0.1	0.5	80	2
13	140	0.2	1	67	2
14	140	0.5	0	129	3
15	140	1	0.1	120	3
16	140	0	0.5	56	1
17	140	0.1	1	60	1
18	140	0.2	0	120	3
19	140	0.5	0.1	122	4
20	140	1	0.2	115	5
21	210	0	1	38	1
22	210	0.1	0	95	2
23	210	0.2	0.1	109	3
24	210	0	0.2	97	5
25	210	1	0.5	89	2

Number	Size of CeO₂/nm	PAAS/% (in mass)	AEO-9/% (in mass)	MRR/(nm·min^-1)	Surface quality
1	110	0	0	71	1
2	110	0.1	0.1	96	3
3	110	0.2	0.2	99	5
4	110	0.5	0.5	79	2
5	110	1	1	70	2
6	110	0	0.1	74	2
7	110	0.1	0.2	100	4
8	110	0.2	0.5	89	2
9	110	0.5	1	66	2
10	110	1	0	120	3
11	140	0	0.2	67	1
12	140	0.1	0.5	80	2
13	140	0.2	1	67	2
14	140	0.5	0	129	3
15	140	1	0.1	120	3
16	140	0	0.5	56	1
17	140	0.1	1	60	1
18	140	0.2	0	120	3
19	140	0.5	0.1	122	4
20	140	1	0.2	115	5
21	210	0	1	38	1
22	210	0.1	0	95	2
23	210	0.2	0.1	109	3
24	210	0	0.2	97	5
25	210	1	0.5	89	2

Number	Size of CeO₂/nm	PAAS/% (in mass)	AEO-9/% (in mass)	MRR/(nm·min^-1)	Surface quality
1	110	0	0	71	1
2	110	0.1	0.1	96	3
3	110	0.2	0.2	99	5
4	110	0.5	0.5	79	2
5	110	1	1	70	2
6	110	0	0.1	74	2
7	110	0.1	0.2	100	4
8	110	0.2	0.5	89	2
9	110	0.5	1	66	2
10	110	1	0	120	3
11	140	0	0.2	67	1
12	140	0.1	0.5	80	2
13	140	0.2	1	67	2
14	140	0.5	0	129	3
15	140	1	0.1	120	3
16	140	0	0.5	56	1
17	140	0.1	1	60	1
18	140	0.2	0	120	3
19	140	0.5	0.1	122	4
20	140	1	0.2	115	5
21	210	0	1	38	1
22	210	0.1	0	95	2
23	210	0.2	0.1	109	3
24	210	0	0.2	97	5
25	210	1	0.5	89	2