三氯化铁-草酸体系不锈钢化学机械抛光液设计与优化

王泽宇; 彭亚男; 苏建修; 陈佳鹏

doi:10.13394/j.cnki.jgszz.2022.0159

三氯化铁-草酸体系不锈钢化学机械抛光液设计与优化

doi: 10.13394/j.cnki.jgszz.2022.0159

王泽宇^1,,
彭亚男²,
苏建修³,
陈佳鹏^{2, 4, ,}

1.
郑州电子信息职业技术学院, 郑州 451450
2.
南京航空航天大学, 江苏省精密与微细制造技术重点实验室, 直升机传动技术国家重点实验室, 南京 210016
3.
河南科技学院机电学院, 河南新乡 453003
4.
上海工程技术大学, 微纳制造先进材料研究中心, 上海 201620

基金项目: 江苏省精密与微细制造技术重点实验室开放基金，国家自然科学基金面上项目(51375149)

详细信息

作者简介:
王泽宇，男，1979年生，讲师。主要研究方向：人工智能大数据处理。E-mail：18738593090@163.com

通讯作者:
陈佳鹏，男，1991年生，讲师、博士、硕士生导师。主要研究方向：超精密加工理论与技术。E-mail：34210007@sues.edu.cn

中图分类号: TG732; TH162; TN27
计量
- 文章访问数: 397
- HTML全文浏览量: 112
- PDF下载量: 38
- 被引次数: 0
出版历程
- 收稿日期: 2022-09-20
- 修回日期: 2022-11-20
- 录用日期: 2022-11-30
- 刊出日期: 2023-08-30

Design and optimization of ferric chloride and oxalic acid based slurry to chemically mechanically polish stainless steel

WANG Zeyu^1
,,
PENG Yanan²,
SU Jianxiu³,
CHEN Jiapeng^{2, 4
, ,}

1.
Zhengzhou Professional Technical Institute of Electronic & Information, Zhengzhou 451450, China
2.
Jiangsu Key Laboratory of Precision and Micro-Manufacturing Technology, National Key Laboratory of Science and Technology on Helicopter Transmission, Nanjing University of Aeronautics and Astronautics, Nanjing 210016, China
3.
School of Mechanical and Electrical Engineering, Henan Institute of Science and Technology, Xinxiang 453003, Henan, China
4.
Research Center for Advanced Micro- / Nano- Fabrication Materials, Shanghai University of Engineering Science, Shanghai 201620, China

摘要

摘要: 为提高柔性显示衬底不锈钢箔片化学机械抛光加工效率，研制一种三氯化铁-草酸型抛光液并用于304不锈钢衬底的化学机械抛光加工过程。设计正交优化试验，确定磨粒粒径、磨料含量、草酸含量和三氯化铁含量对材料去除率和表面粗糙度（S_a）的影响显著性顺序，并重点探究三氯化铁和草酸对材料去除率的影响规律。利用优化后的抛光液精抛304不锈钢，其材料去除率高于560 nm/min，抛光30 min后S_a低于8 nm。相比现有抛光液的材料去除效率（226.56 nm/min），新抛光液的加工效率提升超过1倍。
- 化学机械平坦化 /
- 304不锈钢 /
- 三氯化铁-草酸 /
- 材料去除率 /
- 表面粗糙度
Abstract: To enhance the chemical mechanical polishing (CMP) efficiency of flexible display substrates, a polishing slurry based on ferric chloride and oxalic acid was proposed for polishing 304 stainless steel substrates. An orthogonal optimization test was designed to determine the significance order of the influence of abrasive size, abrasive content, oxalic acid content and ferric chloride content on the material removal rate (MRR) and surface roughness (surface arithmetical mean height of area, S_a). The aim was to investigate the effects of ferric chloride and oxalic acid on MRR. An optimized polishing slurry capable of achieving an MRR of over 560 nm/min and a S_a as low as 8 nm after 30 min was obtain. Compared with the conventional polishing slurry, whose MRR is 226.56 nm/min, the novel slurry has doubled its polishing efficiency or more.
- chemical-mechanical planarization /
- 304 stainless steel /
- ferric chloride-oxalic acid /
- material removal rate /
- surface roughness

HTML全文

图 1 抛光过程的设备(a)和工艺参数(b)

Figure 1. Device (a) and parameters (b) of polishing

下载: 全尺寸图片幻灯片

图 2 抛光液组分对304不锈钢D_MRR(a)和S_a(b)的影响

Figure 2. Effects of polishing slurry components on D_MRR (a) and S_a (b) of 304 stainless steel

下载: 全尺寸图片幻灯片

图 3 磨粒粒径对D_MRR和S_a的显著性分析

Figure 3. Significance analysis for effect of abrasive particle size on D_MRR and S_a

下载: 全尺寸图片幻灯片

图 4 磨料含量对D_MRR和S_a的显著性分析

Figure 4. Significance analysis for effect of abrasive content on D_MRR and S_a

下载: 全尺寸图片幻灯片

图 5 草酸含量对D_MRR和S_a的显著性分析

Figure 5. Significance analysis for oxalic acid content on D_MRR and S_a

下载: 全尺寸图片幻灯片

图 6 三氯化铁含量对D_MRR和S_a的显著性分析

Figure 6. Significance analysis for effect of ferric chloride content on D_MRR and S_a

下载: 全尺寸图片幻灯片

图 7 304不锈钢精抛后的(a)二维和(b)三维表面形貌

Figure 7. 2D (a) and 3D (b) surface morphology of polished 304 stainless steel by optimizational slurry

下载: 全尺寸图片幻灯片

表 1 三氯化铁-草酸型抛光液正交试验

Table 1. Orthogonal test for ferric chloride and oxalic acid type of polishing slurry

水平	因素
	a	b	c	d	e	f
	粒	磨料质	分散剂	草酸质	三氯化铁	活性剂
	径	量分数	质量分数	量分数	质量分数	质量分数
	d / μm	w_g / %	w_d / %	w_o / %	w_f / %	w_a / %
1	0.5	0.8	0.4	0.4	2	0.04
2	7.0	4.0	1.2	0.8	6	0.20
3	14.0	7.2	2.0	1.2	10	0.40
4	28.0	9.6	2.8	1.6	14	0.80

下载: 导出CSV

表 2 三氯化铁-草酸型抛光液组分优化试验数据表

Table 2. Experimental data for ferric chloride and oxalic acid type of polishing slurry optimization

序号	a	b	c	d	e	f	D_MRR nm/min	S_a nm
1	0.5	0.8	0.4	0.4	2	0.04	325.3	13
2	0.5	4.0	1.2	0.8	6	0.20	558.6	11
3	0.5	7.2	2.0	1.2	10	0.40	502.3	8
4	0.5	9.6	2.8	1.6	14	0.80	430.2	9
5	7.0	0.8	0.4	0.8	6	0.40	495.2	12
6	7.0	4.0	1.2	0.4	2	0.80	486.2	29
7	7.0	7.2	2.0	1.6	14	0.04	509.5	21
8	7.0	9.6	2.8	1.2	10	0.20	533.6	19
9	14.0	0.8	1.2	1.2	14	0.4	503.5	19
10	14.0	4.0	0.4	1.6	10	0.20	595.6	17
11	14.0	7.2	2.8	0.4	6	0.04	605.6	36
12	14.0	9.6	2.0	0.8	2	0.80	560.7	23
13	28.0	0.8	1.2	1.6	10	0.40	588.3	29
14	28.0	4.0	0.4	1.2	14	0.80	624.3	27
15	28.0	7.2	2.8	0.8	2	0.04	617.4	36
16	28.0	9.6	2.0	0.4	6	0.20	674.4	23
17	0.5	0.8	2.8	0.4	14	0.20	402.7	13
18	0.5	4.0	2.0	0.8	10	0.04	550.3	11
19	0.5	7.2	1.2	1.2	6	0.80	502.4	8
20	0.5	9.6	0.4	1.6	2	0.40	389.1	9
21	7.0	0.8	2.8	0.8	10	0.80	502.3	12
22	7.0	4.0	2.0	0.4	14	0.40	548.7	29
23	7.0	7.2	1.2	1.6	2	0.20	483.7	21
24	7.0	9.6	0.4	1.2	6	0.04	518.6	19
25	14.0	0.8	2.0	1.2	2	0.20	520.7	19
26	14.0	4.0	2.8	1.6	6	0.04	641.3	17
27	14.0	7.2	0.4	0.4	10	0.80	537.8	36
28	14.0	9.6	1.2	0.8	14	0.40	565.6	23
29	28.0	0.8	2.0	1.6	6	0.80	563.4	29
30	28.0	4.0	2.8	1.2	2	0.40	576.8	27
31	28.0	7.2	0.4	0.8	14	0.20	551.3	36
32	28.0	9.6	1.2	0.4	10	0.04	541.7	23

下载: 导出CSV

表 3 抛光液各组分对MRR的影响显著性分析

Table 3. Significance analysis for effect of each component of polishing slurry on MRR

因素	自由度	离均差平方和	均方和	F	P_r > F
a	3	259 966.862 5	86 655.621	192.93	<0.000 1
b	3	88 715.559 4	29 571.853	65.84	<0.000 1
c	3	30 639.930 0	10 213.310	22.74	<0.000 1
d	3	15 975.215 5	5 325.072	11.86	<0.000 1
e	3	76 268.718 9	25 422.906	56.60	<0.000 1
f	3	3 389.954 0	1 129.985	2.52	0.064 5

下载: 导出CSV

表 4 抛光液各组分对S_a的影响显著性分析

Table 4. Significance analysis for effect of each component of polishing slurry on S_a

因素	自由度	离均差平方和	均方和	F	P_r > F
a	3	0.004 404 00	0.001 468 00	68.44	<0.000 1
b	3	0.000 759 00	0.000 253 00	11.80	<0.000 1
c	3	0.000 013 50	0.000 004 50	0.21	0.889 3
d	3	0.000 711 00	0.000 237 00	11.05	<0.000 1
e	3	0.000 181 50	0.000 0605 0	2.82	0.044 4
f	3	0.000 073 50	0.000 0245 0	1.14	0.337 4

下载: 导出CSV

参考文献(20)

[1]	ERITT M, MAY C, LEO K, et al. OLED manufacturing for large area lighting applications [J]. Thin Solid Films,2010,518(11):3042-3045. doi: 10.1016/j.tsf.2009.09.188
[2]	GUSTAFSSON G, CAO Y, TREACY G M, et al. Flexible light-emitting diodes made from soluble conducting polymers [J]. Nature,1992,357(6378):477-479. doi: 10.1038/357477a0
[3]	LEWIS J S, WEAVER M S. Thin-film permeation-barrier technology for flexible organic light-emitting devices [J]. IEEE Journal of Selected Topics in Quantum Electronics,2004,10(1):45-57. doi: 10.1109/JSTQE.2004.824072
[4]	YUAN Y Y, HAN S, GROZEA D, et al. Fullerene-organic nanocomposite: A flexible material platform for organic light-emitting diodes [J]. Applied Physics Letters,2006,88(9):093503. doi: 10.1063/1.2180876
[5]	CHWANG A B, ROTHMAN M A, MAO S Y, et al. Thin film encapsulated flexible organic electroluminescent displays [J]. Applied Physics Letters,2003,83(3):413-415. doi: 10.1063/1.1594284
[6]	HANANDA T, NEGISHI T, SHIROISHI I, et al. Plastic substrate with gas barrier layer and transparent conductive oxide thin film for flexible displays [J]. Thin Solid Films,2010,518(11):3089-3092. doi: 10.1016/j.tsf.2009.09.166
[7]	杨利营, 印寿根, 华玉林, 等. 柔性显示器件的衬底材料及封装技术 [J]. 功能材料,2006(1):10-13. YANG Liying, YIN Shougen, HUA Yulin, et al. Flexible substrates and encapsulation methods for flexible organic light emitting devices [J]. Jorunal of Functional Materials,2006(1):10-13.
[8]	冯魏良, 黄培. 柔性显示衬底的研究及进展 [J]. 液晶与显示,2012,27(5):599-607. doi: 10.3788/YJYXS20122705.0599 FENG Weiliang, HUANG Pei. Advances in flexible displays substrates [J]. Chinese Journal of Liquid Crystals and Displays,2012,27(5):599-607. doi: 10.3788/YJYXS20122705.0599
[9]	AUCH M D J, SOO O K, EWALD G, et al. Ultrathin glass for flexible OLED application [J]. Thin solid films,2002,417(1):47-50.
[10]	廖显杰. 柔性显示的“面子”和“里子”−谈基板材料的发展现状与趋势 [J]. 中国数字电视,2007(Z1):84-87. LIAO Xianjie. The "surface" and "inside" of flexible display: The development status and trend of substrate materials [J]. China Digital TV,2007(Z1):84-87.
[11]	刘海旭, 武庆东, 曹潇俊, 等. 基于响应曲面法的304不锈钢化学机械抛光工艺参数优化 [J]. 金刚石与磨料磨具工程,2021,41(2):89-95. LIU Haixu, WU Qingdong, CAO Xiaojun, et al. Prediction and optimization of process parameters in chemical mechanical polishing for 304 stainless steel based on response surface methodology [J]. Diamond & Abrasives Engineering,2021,41(2):89-95.
[12]	李庆, 陈绍坤, 彭亚男, 等. 304不锈钢化学机械抛光工艺参数研究 [J]. 金刚石与磨料磨具工程,2016,36(5):21-25. LI Qing, CHEN Shaokun, PENG Yanan, et al. Chemical mechanical polishing process parameters of 304 stainless steel [J]. Diamond & Abrasives Engineering,2016,36(5):21-25.
[13]	秦洪权, 王永胜, 李庆, 等. 化学机械抛光超薄SUS304不锈钢抛光液研究 [J]. 金刚石与磨料磨具工程,2016,36(6):25-28+34. QIN Hongquan, WANG Yongsheng, LI Qing, et al. Polishing slurry of chemical mechanical polishing SUS304 ultrathin stainless steel sheet [J]. Diamond & Abrasives Engineering,2016,36(6):25-28+34.
[14]	HU X, SONG Z, LIU W, et al. Chemical mechanical polishing of stainless steel foil as flexible substrate [J]. Applied Surface Science,2012,258(15):5798-5802. doi: 10.1016/j.apsusc.2012.02.100
[15]	杨向东, 魏昕, 谢小柱, 等. 基于化学机械抛光过程的超薄不锈钢基板表面特性分析 [J]. 润滑与密封,2015,40(4):45-48+53. YANG Xiangdong, WEI Xin, XIE Xiaozhu, et al. Analysis of surface characteristics of ultra-thin stainless steel substrate based on chemical mechanical polishing process [J]. Lubrication Engineering,2015,40(4):45-48+53.
[16]	刘振辉, 陈绍坤, 彭亚男, 等. 化学机械抛光304不锈钢用抛光液成分研究 [J]. 金刚石与磨料磨具工程,2018,38(2):78-81+88. LIU Zhenhui, CHEN Shaokun, PENG Yanan, et al. Compositions of slurry used in chemical-mechanical polishing 304 stainless steel [J]. Diamond & Abrasives Engineering,2018,38(2):78-81+88.
[17]	张仁杰, 张振宇, 李玉彪, 等. 304不锈钢绿色化学机械抛光 [J]. 表面技术,2022,51(5):325-335. ZHANG Renjie, ZHANG Zhenyu, LI Yubiao, et al. Green chemical mechanical polishing of 304 stainless steel [J]. Surface Technology,2022,51(5):325-335.
[18]	崔洪刚, 汪永超, 唐浩. 不锈钢CMP抛光液的研制 [J]. 机械设计与制造,2018(1):73-75. doi: 10.19356/j.cnki.1001-3997.2018.01.021
[19]	王浩, 陈国美, 倪自丰, 等. 1, 2, 4–三氮唑和苯并三氮唑对316L不锈钢化学机械抛光的影响 [J]. 金刚石与磨料磨具工程,2021,41(1):83-88. WANG Hao, CHEN Guomei, NI Zifeng, et al. Effect of 1, 2, 4 - triazole and benzotriazole on chemical-mechanical polishing of 316L stainless steel [J]. Diamond & Abrasives Engineering,2021,41(1):83-88.
[20]	陈佳鹏, 陈绍坤, 李庆, 等. 用碱性抛光液化学机械抛光304不锈钢片研究 [J]. 金刚石与磨料磨具工程,2016,36(2):6-9+23. CHEN Jiapeng, CHEN Shaokun, LI Qing, et al. Study on chemical mechanical polishing 304 stainless steel sheet based on alkaline polishing slurry [J]. Diamond & Abrasives Engineering,2016,36(2):6-9+23.