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Volume 45 Issue 1
Mar.  2025
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Article Navigation >  Diamond & Abrasives Engineering  > 2025  >  45(1): 113-121
CHENG Feng, WANG Zirui, ZHU Rui, WANG Yongguang, PENG Yang, ZHANG Tianyu, ZHAO Dong, FAN Cheng. Study on dispersion of abrasive particles in electro Fenton CMP slurry and design of green polishing fluid in neutral environment[J]. Diamond & Abrasives Engineering, 2025, 45(1): 113-121. doi: 10.13394/j.cnki.jgszz.2023.0242
Citation: CHENG Feng, WANG Zirui, ZHU Rui, WANG Yongguang, PENG Yang, ZHANG Tianyu, ZHAO Dong, FAN Cheng. Study on dispersion of abrasive particles in electro Fenton CMP slurry and design of green polishing fluid in neutral environment[J]. Diamond & Abrasives Engineering, 2025, 45(1): 113-121. doi: 10.13394/j.cnki.jgszz.2023.0242
shu

Study on dispersion of abrasive particles in electro Fenton CMP slurry and design of green polishing fluid in neutral environment

doi: 10.13394/j.cnki.jgszz.2023.0242

  • School of Mechanical and Electrical Engineering, Soochow University, Suzhou 215021, Jiangsu, China

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  • Received Date: 2023-11-15
  • Accepted Date: 2024-04-18
  • Rev Recd Date: 2024-02-06
    • Available Online: 2025-03-24
    Abstract
  •   Objectives  In the process of GaN ultra-precision polishing, diamond abrasives tend to agglomerate, leading to an increase in the average particle size of abrasives in the polishing slurry, which negatively impacts the surface precision of GaN. The addition of Fe2+ in the Fenton reaction exacerbates this phenomenon. To address this issue, adding electrolytes to the polishing slurry has proven effective in mitigating the agglomeration and sedimentation of abrasives. To compare the effects of STPP, NaCl, and Na2SO4 on the dispersion stability of diamond abrasives during the Fenton reaction, the citric acid and the sodium hydroxide are used as pH regulators to investigate the Fenton reaction of green polishing solution at different pH values. The effects on the anti-settling ability of diamond abrasive particles, the Zeta potential of polishing slurry, and the polishing solution abrasive particle size are studied, and the polishing effect on the GaN wafer is verified.  Methods  Nano-diamond abrasive particles with an average particle size of 180 nm were added to deionized water, and H2O2 with a mass fraction of 5% and FeSO4·7H2O with a mass of 0.2 g were added as the original reactants of the Fenton reaction. Then, NaCl, Na2SO4 and STPP electrolytes with a mass fraction of 1% were added to prepare three groups of Fenton reaction polishing slurry, which were compared with the original Fenton reaction polishing slurry without any additional electrolyte. After thorough stirring for 5 minutes and ultrasonic dispersion for 10 minutes, citric acid and sodium hydroxide were used to adjust the pH values of all four slurries to 3. At the same time, the polishing slurry with STPP electrolyte at a pH value of 6 was prepared, and the influence of pH value on the anti-settling effect of diamond abrasive particles under STPP electrolyte was preliminarily investigated as the control group. The above five groups of polishing slurries were added to glass bottles for particle settling experiments, and the dispersion stability of diamond abrasive particles in different groups of polishing slurry was observed. The Zetasizer Nano ZS90 nanometer particle size potential analyzer was used to measure the Zeta potential and the particle size of the five groups of polishing slurries before and after the addition of a pH regulator. Finally, the ECMP experiment was carried out to study the effects of green polishing slurries on material removal rate and surface roughness at different pH values.  Results  (1) When the pH value is 3, the original Fenton polishing slurry and the polishing slurries with NaCl and Na2SO4 electrolytes have weaker anti-settling ability compared to the polishing slurry with STPP added, and the effect of improving the anti-settling ability of diamond abrasives is not obvious. The first three groups of polishing slurries exhibit an obvious delamination phenomenon at the bottom within the first 10 minutes. This indicates that STPP can improve the anti-settling ability of diamond abrasives in Fenton reaction polishing slurry. Furthermore, comparing the polishing slurry samples with STPP added at pH values of 3 and 6, it is found that the anti-settling ability of diamond in the polishing slurry with a pH value of 3 is significantly lower than that in the sample with a pH value of 6, indicating that STPP can improve the anti-settling ability of diamond abrasives in an environment with a pH value of 6. (2) The addition of NaCl and Na2SO4 electrolytes results in a smaller absolute Zeta potential and poorer stability of the polishing slurry, while the addition of STPP greatly increases the dispersion stability of diamond abrasives in the Fenton reaction polishing slurry. At the same time, after adjusting the pH value to 3, the absolute values of the Zeta potential of all polishing slurries slightly decrease compared to before pH adjustment, indicating a decrease in the stability of the polishing slurry. That is, the addition of acidic electrolytes may reduce the stability of the polishing slurry. (3) When the surface of GaN is processed with the polishing slurry containing STPP, there are almost no deep scratches caused by abrasive agglomeration compared with other comparison groups. The surface quality of the processed GaN is the best, with a surface roughness Ra as low as 0.449 nm, and the material removal rate is much higher than that of the control group, reaching up to 705.3 nm/h.  Conclusions  The Fenton reaction utilizes Fe2+ to react with H2O2 to generate hydroxyl radicals (·OH) with strong oxidizing properties. With the addition of STPP, Fe2+in the solution forms a relatively stable complex Fe2+-STPP with STPP, and which quickly reacts with H2O2 to form Fe3+-STPP and ·OH after the addition of H2O2, effectively avoiding the presence of a large amount of free Fe3+ and the precipitation of Fe(OH)3. Adding STPP to the Fenton reaction polishing slurry with diamond as abrasive particles can broaden the pH range of the Fenton reaction polishing slurry, breaking the limit of pH≤3, and preventing the precipitation of iron flocs in the polishing slurry in a neutral environment. Meanwhile, STPP can enhance the anti-settling ability of diamond abrasives in the Fenton reaction polishing slurry in a neutral environment, and the alkaline pH regulator weakens the anti-settling ability of diamond abrasives in polishing slurry more significantly than the acidic pH regulator.

     

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