Taguchi’s method was applied to investigate the effect of main high energy ball milling (HEBM) parameters: milling time (MT), ball to powder weight ratio (BPWR), and milling speed (MS) on the CaCO3 crystallite size. The settings of HEBM parameters were determined by using the L9 (33) orthogonal experiments array (OA). The as-received and milled powders were characterized by X-ray diffraction (XRD) scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy. The crystallite size of CaCO3 varied between 140 and 540 nm depending on the HEBM conditions. The analysis of variance (ANOVA) was used to find the significance and percentage of contribution of each milling parameter. It was established that the MT is the most effective parameter followed by MS and BPWR. A confirmation test was carried out with a 90% confidence level to illustrate the effectiveness of the Taguchi optimization method. The optimum milling parameter combination was determined by using the analysis of signal-to-noise (S/N) ratio. Based on the S/N ratio analysis, optimal HEBM conditions were found MT 10 h, MS 600 revolutions per minute (rpm), BPWR 50:1.

中文翻译：

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田口法高能球磨CaCO3的应用

田口的方法用于研究主要高能球磨 (HEBM) 参数：研磨时间 (MT)、球粉重量比 (BPWR) 和研磨速度 (MS) 对 CaCO3 微晶尺寸的影响。HEBM 参数的设置通过使用 L9 (33) 正交实验阵列 (OA) 确定。通过 X 射线衍射 (XRD) 扫描电子显微镜 (SEM)、傅里叶变换红外 (FTIR) 光谱对原样和研磨的粉末进行表征。CaCO3 的微晶尺寸在 140 到 540 nm 之间变化，具体取决于 HEBM 条件。方差分析 (ANOVA) 用于找出每个研磨参数的显着性和贡献百分比。已确定 MT 是最有效的参数，其次是 MS 和 BPWR。以 90% 的置信度进行了确认测试，以说明田口优化方法的有效性。通过对信噪比（S/N）的分析确定了最佳铣削参数组合。基于信噪比分析，发现最佳 HEBM 条件为 MT 10 小时、MS 600 转每分钟 (rpm)、BPWR 50:1。