目的 探究一种新型的可见光催化SiC化学机械抛光方法,实现单晶SiC在可见光照射下的高效、超精密加工。方法 通过甲基橙褪色实验,电化学实验,浸泡腐蚀实验以及抛光实验,分析不同反应体系（Fe3+/H2O2、Vis/TiO2/H2O2、Vis/WO3/H2O2、Vis/TiO2/Fe3+/H2O2、Vis/WO3/Fe3+/H2O2）抛光液的氧化性以及对SiC抛光效果的影响,揭示基于WO3/Fe3+的可见光催化SiC化学机械抛光机理。在最佳反应体系条件（Vis/WO3/Fe3+/H2O2）下,引入金刚石/SiO2混合磨料,通过有无光源的抛光对比实验,初步验证金刚石/SiO2混合磨料可见光催化SiC抛光的可行性。结果 在5种不同反应体系溶液中,Vis/WO3/Fe3+/H2O2反应体系溶液的甲基橙褪色时间最短、电化学腐蚀电位最大,浸泡腐蚀后SiC表面氧元素含量（原子数分数）最高（9.48%）,溶液氧化性最强,在该反应体系下使用SiO2磨料抛光SiC的材料去除率为279.83 nm/h,表面粗糙度Sa为55.73 nm,抛光效果最好。相较于无光源的金刚石/SiO2混合磨料SiC抛光,有光源的SiC抛光效果更好,材料去除率进一步提高,抛光0.5 h后,表面粗糙度Sa由120 nm显著降低至0.861 nm。结论 在可见光的照射下,Fe3+有利于WO3光催化效率的提高,形成了可见光催化反应与芬顿反应的协同作用,显著提升了抛光液对SiC的氧化能力和抛光效果,同时,初步验证了金刚石/SiO2混合磨料在可见光催化体系下抛光SiC的可行性,获得了材料去除率高和表面质量较好的SiC晶片。
Abstract
The work aims to explore a new visible-light-catalyzed chemical and mechanical polishing method for SiC, to achieve efficient and ultra-precise processing of single-crystal SiC under visible light irradiation. The oxidizing properties of polishing solutions in different reaction systems (Fe3+/H2O2, Vis/TiO2/H2O2, Vis/WO3/H2O2, Vis/TiO2/Fe3+/H2O2, Vis/WO3/Fe3+/H2O2) were systematically analyzed through methyl orange decolorization experiments, electrochemical tests, immersion corrosion experiments, and polishing experiments, combined with detection results from instruments such as an electrochemical workstation, scanning electron microscope (SEM), X-ray energy dispersive spectrometer (EDS), and X-ray photoelectron spectroscope (XPS). The removal rate of SiC polishing materials was calculated with the weight loss method, and the surface roughness and morphology of polished SiC were obtained via a 3D surface profiler. The effects of polishing solutions from different reaction systems on the removal rate of SiC polishing materials and surface quality were investigated, revealing the mechanism of visible-light-catalyzed chemical and mechanical polishing of SiC based on WO3/Fe3+. Under the optimal reaction system conditions (Vis/WO3/Fe3+/H2O2), diamond/SiO2 mixed abrasives were further introduced. Through comparative experiments of polishing SiC with or without a light source (wavelength 425 nm), the feasibility of polishing visible-light-catalyzed SiC with diamond/SiO2 mixed abrasives was preliminarily verified. Experimental results showed that among the five different reaction system solutions, the Vis/WO3/Fe3+/H2O2 reaction system solution had the shortest decolorization time for methyl orange, the highest electrochemical corrosion potential, and the highest oxygen content on the SiC surface after immersion corrosion (9.48at.%), indicating the strongest oxidative ability of the solution. Under this reaction system, using SiO2 abrasive to polish SiC resulted in a material removal rate of 279.83 nm/h and a surface roughness Sa of 55.73 nm, achieving the best polishing effect compared to the other reaction systems. In the comparative experiment of polishing SiC with diamond/SiO2 mixed abrasives under conditions with and without visible light, the polishing effect of diamond/SiO2 mixed abrasives under visible light was better, with a further increase in material removal rate. After 0.5 hours of polishing, the surface roughness Sa of SiC significantly decreased from 120 nm to 0.861 nm. Analysis of the experimental results showed that under visible light irradiation, Fe3+ promoted the visible light photocatalytic reaction. Compared with the TiO2 photocatalyst, Fe3+ had a more significant promoting effect on the visible light photocatalytic reaction of WO3. The Fe3+ reacted with photogenerated electrons in the conduction band of WO3, reducing Fe3+ to Fe2+, which greatly decreased the recombination of WO3 photogenerated electron-hole pairs and enhanced the photocatalytic efficiency of WO3. At the same time, the generated Fe2+ underwent a Fenton reaction with H2O2 in the solution, creating a synergistic effect between visible light photocatalysis and the Fenton reaction. This increased the concentration of highly oxidative hydroxyl radicals in the polishing solution, significantly improving the oxidation ability and polishing effect of the solution on SiC. Through comparative experiments of SiC polishing under conditions with and without visible light, the feasibility of polishing SiC with diamond/SiO2 mixed abrasives in a Vis/WO3/Fe3+/H2O2 visible light catalytic reaction system was preliminarily verified. By combining the chemical action of the polishing slurry under visible light catalysis with the mechanical action of the diamond/SiO2 mixed abrasives, SiC wafers with high material removal rates and relatively good surface quality were obtained.
关键词
SiC /
WO3 /
可见光催化 /
Fe3+ /
羟基自由基 /
化学机械抛光
Key words
SiC /
WO3 /
visible light photocatalysis /
Fe3+ /
hydroxyl radical /
chemical and mechanical polishing
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基金
浙江省自然科学基金（LQ23E050003）; 国家自然科学基金（面上52475446,海外2023）; 安徽省自然科学基金项目（面上2308085ME170）; 安徽省科技创新攻坚计划重大重点项目（202423i08050035）; 温州市重大科技创新攻关项目（ZG2022029）
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