Application of the Taguchi and ANOVA methods to optimize high-energy ball milling parameters for dislocation density of TiO2 powder

Due to its particular properties, titanium dioxide (TiO₂) has been widely used in industry. In this study, the high-energy ball milling (HEBM) parameters, including milling time (MT), ball-to-powder weight ratio (BPWR), and milling speed (MS), have been optimized using the Taguchi method.

TiO₂ dislocation density (DD) was used to estimate the effect of the HEBM. The experiment was applied using the 𝐿16(4³) orthogonal array (OA). The as-received and milled powders were characterized by X-ray diffraction (XRD). The DD, determined by the Williamson-Hall (W-H) method in XRD patterns, varied between 0.02⋅ 10⁻² − 8.26 ⋅ 10⁻² lines/nm² depending on the HEBM conditions. The optimum milling parameter combination was determined by analysis of signal-to-noise (S/N) ratio. Based on the S/N ratio analysis, optimal HEBM conditions were found at MT 50h, MS 600rpm, BPWR 50:1. The analysis of variance (ANOVA) was used to find the significance and percentage of contribution of each milling parameter. Statistical analysis by S/N and ANOVA established that the MT was the most effective parameter, followed by MS and BPWR. The results of the parameter optimization experiments were validated by a confirmation test with a 90% confidence level.