白西郁,李薇薇,钟荣峰,肖银波,王晓剑,许宁徽.钽晶圆CMP抛光液成分与加工工艺参数的研究与优化[J].表面技术,2024,53(24):133-143.
BAI Xiyu,LI Weiwei,ZHONG Rongfeng,XIAO Yinbo,WANG Xiaojian,XU Ninghui.Research and Optimization of Composition and Processing Parameters of Tantalum Crystal Wafer CMP Polishing Slurry[J].Surface Technology,2024,53(24):133-143 |
| 钽晶圆CMP抛光液成分与加工工艺参数的研究与优化 |
| Research and Optimization of Composition and Processing Parameters of Tantalum Crystal Wafer CMP Polishing Slurry |
| 投稿时间：2024-03-06 修订日期：2024-07-03 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.24.012 |
| 中文关键词: 钽晶圆 化学机械抛光 电化学 响应面法 材料去除速率 表面粗糙度 |
| 英文关键词:tantalum wafers chemical mechanical polishing electrochemistry response surface methodology material removal rate surface roughness |
| 基金项目:国家自然科学基金(62275073) |
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| Author | Institution |
| BAI Xiyu | College of Electronic Information Engineering, Hebei University of Technology, Tianjin 300401, China |
| LI Weiwei | College of Electronic Information Engineering, Hebei University of Technology, Tianjin 300401, China |
| ZHONG Rongfeng | Guangdong Wellt-Nanotech Co., Ltd., Guangdong Dongguan 523000, China |
| XIAO Yinbo | Guangdong Wellt-Nanotech Co., Ltd., Guangdong Dongguan 523000, China |
| WANG Xiaojian | College of Electronic Information Engineering, Hebei University of Technology, Tianjin 300401, China |
| XU Ninghui | College of Electronic Information Engineering, Hebei University of Technology, Tianjin 300401, China |
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| 中文摘要: |
| 目的 通过电化学实验确定化学机械抛光液成分，并以此进行化学机械抛光实验，通过响应面法确定最佳工艺参数方案。方法 通过电化学实验结果确定甘氨酸和过硫酸钠、过氧化氢2种氧化剂的最佳组合与配比，以此配制抛光液进行不同机械参数的CMP实验，选择抛光压力、抛光盘转速、抛光液流3种工艺参数，取值分别为6.5~9.5 kg、30~90 r/min、45~105 mL/min，利用响应面实验法确定最佳工艺参数组合方案。结果 通过电化学实验确定抛光液组分甘氨酸质量分数为0.3%、H2O2质量分数为3%，应用响应面法确定的抛光压力、抛光盘转速、抛光液流量分别为8.1 kg、70 r/min、79 mL/min，分析得到各工艺参数按对抛光效果的影响程度从强到弱依次为:抛光压力、抛光盘转速、抛光液流量。最终钽晶圆实验材料去除速率为29.445 nm/min，具有良好的表面质量，其表面粗糙度为0.152 nm。结论 甘氨酸能够降低腐蚀速率，氧化剂能够加速钽腐蚀速率，混合电化学实验结果表明，甘氨酸也可以减缓氧化剂对钽腐蚀的促进作用，因此甘氨酸可与氧化剂配合使用来控制对钽的腐蚀。使用响应面分析法可以确定最佳工艺参数方案，所以采用响应面分析法可以降低实验成本，提高实验效率。 |
| 英文摘要: |
| Tantalum wafer chemical mechanical polishing (CMP) is a key process in semiconductor manufacturing. The work aims to achieve a highly planar and smooth surface texture on the tantalum wafer. The effectiveness of CMP was determined by the combined effects of chemical corrosion and mechanical abrasion. In this study, electrochemical experiments were conducted to determine the optimal combination and ratio of glycine and persulfate, with hydrogen peroxide as oxidants. The experiments utilized the Wuhan correst CS310M electrochemical workstation, with a mercury-oxidized mercury electrode as the reference, a platinum electrode as the auxiliary, and a tantalum electrode (with an exposed area of 1 cm²) as the working electrode. The optimal combination was found to be a mixture of glycine and hydrogen peroxide, with mass fractions of 0.3 wt.% and 3 wt.%, respectively, resulting in a corrosion rate of 0.005 62 mm/a. Subsequently, to establish the optimal range of process parameters for subsequent response surface experiments, single-factor CMP experiments were conducted using the electrochemically determined polishing solution. The process parameters tested were polishing pressure, polishing disc rotation speed, and polishing fluid flow rate, with values ranging from 6.5 to 9.5 kg, 30 to 90 r/min, and 45 to 105 mL/min, respectively. The experiments were performed on a 1-inch diameter, 1 000 μm thick tantalum wafer that underwent preliminary grinding using the UNIPOL-1200S automatic polishing machine, with a GL-86 type velvet polishing pad. The optimal ranges for the polishing pressure, polishing disc rotation speed, and polishing fluid flow rate were determined to be 7 to 9 kg, 50 to 70 r/min, and 65 to 85 mL/min, respectively. Additionally, response surface experiments were designed based on the ranges determined by the single-factor experiments. CMP experiments were carried out according to the response surface experimental design, and the results were input into Design-Expert 13 software to establish a mathematical predictive model and plot response surface graphs. The model was validated to be effective and reasonable. Analysis of the response surface graphs revealed that the degree of influence on the polishing effect, from highest to lowest, was polishing pressure, polishing disc rotation speed, and polishing fluid flow rate. Therefore, the emphasis should be placed on adjusting the polishing pressure in the polishing experiments. The interaction between polishing pressure and polishing disc rotation speed significantly influenced the polishing effect, while the interaction between polishing pressure and polishing fluid flow rate, as well as the interaction between polishing disc rotation speed and polishing fluid flow rate, were not significant. Based on the mathematical model, the optimal process parameter combination was predicted, with a polishing pressure of 8.1 kg, a polishing disc rotation speed of 70 r/min, and a polishing fluid flow rate of 79 mL/min. Under these conditions, the achieved material removal rate and surface roughness were 29.445 nm/min and 0.152 nm, respectively. The study ultimately determines that glycine can slow down the corrosion rate, while oxidants can accelerate the corrosion rate of tantalum. Mixed electrochemical experiments show that glycine can also mitigate the promoting effect of oxidants on the corrosion of tantalum. Therefore, glycine can be used in conjunction with oxidants to control the corrosion of tantalum. The use of response surface analysis can determine the optimal process parameter scheme, yielding favorable polishing effects, thereby reducing experimental costs and improving experimental efficiency. |
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