Amorphous silicon nanomaterial is isotropic on the macroscale and can effectively inhibit the expansion/contraction during lithiation/delithiation processes, which remarkably improves the cycle performance of Li-ion batteries. Bead-milling is a simple, cost-effective, and scalable method for manufacturing amorphous and/or crystalline silicon nanoparticles. In this work, the internal structure of Si nanoparticles prepared by bead-milling was found to consist of amorphous and nanocrystalline silicon as well as amorphous silicon oxide. X-ray diffraction patterns and Raman spectra are used to calculate the average crystallite size and estimate the degree of crystallization and amorphization of silicon. The quantitative analysis of amorphous silicon oxide is carried out through x-ray photoelectron spectroscopy characterization and oxygen content measuring. It was found that the average particle size (D₅₀) and the crystallite size were reduced to 91 and 3.7 nm, respectively, from 4.06 μm and 50.6 nm before bead-milling, and the degree of amorphization and oxygen content increased to 85.7% and 7.38%, respectively, from 37.5% and 0.12% before bead-milling. It is demonstrated that the longer the milling time, the smaller the sizes of particles and crystals and the higher the ratio of the amorphous phase. However, it inversely causes side-effects such as the increase in oxidization of Si nanoparticles and the increase in content of ZrO₂ impurity.

中文翻译：

---

通过珠磨法开发的硅纳米粒子的内部结构的形成和定量分析

非晶硅纳米材料在宏观上具有各向同性，可有效抑制锂化/脱锂过程中的膨胀/收缩，显着提高锂离子电池的循环性能。珠磨是一种用于制造非晶和/或晶体硅纳米粒子的简单、经济且可扩展的方法。在这项工作中，发现通过珠磨制备的硅纳米粒子的内部结构由非晶硅和纳米晶硅以及非晶氧化硅组成。X 射线衍射图和拉曼光谱用于计算平均微晶尺寸并估计硅的结晶度和非晶化程度。通过X射线光电子能谱表征和氧含量测量对非晶氧化硅进行定量分析。发现平均粒径（D₅₀ ) 和微晶尺寸分别从珠磨前的4.06 μ m 和 50.6 nm减小到 91 nm 和 3.7 nm，并且非晶化程度和氧含量分别从 37.5% 和 7.38% 提高到 85.7% 和 7.38%珠磨前 0.12%。结果表明，球磨时间越长，颗粒和晶体的尺寸越小，非晶相的比例越高。然而，它反过来会导致诸如Si纳米颗粒氧化增加和ZrO ₂杂质含量增加等副作用。