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[求助]
如何通过xrd实验得到晶粒尺寸？xrd 实验中如何去除仪器展宽得到样品的半峰宽？ 已有1人参与
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最近在修改论文遇到了一个比较紧急的问题，在进行xrd测试时，仅仅测试了样品的xrd谱线。随后用得到的数据在jade软件上拟合处理，得出FWHM。但是期刊审稿人要求考虑仪器展宽的影响，得到样品本身的FWHM，再计算晶粒尺寸大小。这个问题该如何处理？大佬们有推荐的参考资料嘛？ @lich666 @jackdeng 发自小木虫IOS客户端 |
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rlafite
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3楼2025-07-09 00:14:59
rlafite
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Williamson-Hall Method The Williamson-Hall (W-H) method is a technique used in X-ray diffraction (XRD) analysis to estimate crystallite size and microstrain within a material. It's based on the principle that peak broadening in XRD patterns is influenced by both the size of the crystallites and the strain within the crystal lattice. By plotting broadening parameters against diffraction angle, the W-H method allows researchers to differentiate between these two contributions and obtain quantitative values for both size and strain. Here's a more detailed explanation: 1. Peak Broadening in XRD: XRD patterns show peaks at specific angles (2θ) that correspond to the crystal structure of the material. These peaks have a certain width, which is influenced by both the instrument used for measurement and the material itself. Instrumental broadening is a fixed factor for a given setup, while sample-related broadening is caused by factors like small crystallite size and lattice strain. 2. Williamson-Hall Method: The W-H method focuses on separating the size-related and strain-related broadening components. It utilizes a plot where the x-axis represents sin θ (where θ is half of the diffraction angle 2θ) and the y-axis represents βcos θ (where β is the full width at half maximum (FWHM) of the diffraction peak). This plot is based on the equation: βcos θ = (Kλ/D) + 4εsin θ. β is the FWHM of the diffraction peak. θ is the Bragg angle. K is a dimensionless shape factor (typically around 0.9). λ is the wavelength of the X-ray radiation. D is the average crystallite size. ε is the microstrain. 3. Analyzing the W-H Plot: The plot should ideally be linear. The slope of the line represents the microstrain (ε). The y-intercept of the line provides information to calculate the average crystallite size (D). By analyzing the slope and intercept, researchers can estimate both the size of the crystallites and the strain within them. In essence, the W-H method provides a relatively simple way to extract information about the microstructure of materials from XRD data, specifically by separating and quantifying the effects of crystallite size and lattice strain |
2楼2025-07-08 23:02:09
