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大可樂(lè)hcl新蟲(chóng) (初入文壇)
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[求助]
如何通過(guò)xrd實(shí)驗(yàn)得到晶粒尺寸？xrd 實(shí)驗(yàn)中如何去除儀器展寬得到樣品的半峰寬？ 已有1人參與
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最近在修改論文遇到了一個(gè)比較緊急的問(wèn)題，在進(jìn)行xrd測(cè)試時(shí)，僅僅測(cè)試了樣品的xrd譜線。隨后用得到的數(shù)據(jù)在jade軟件上擬合處理，得出FWHM。但是期刊審稿人要求考慮儀器展寬的影響，得到樣品本身的FWHM，再計(jì)算晶粒尺寸大小。這個(gè)問(wèn)題該如何處理？大佬們有推薦的參考資料嘛？ @lich666 @jackdeng 發(fā)自小木蟲(chóng)IOS客戶端 |
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rlafite
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3樓2025-07-09 00:14:59
rlafite
木蟲(chóng) (正式寫(xiě)手)
- 應(yīng)助: 190 (高中生)
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【答案】應(yīng)助回帖
感謝參與，應(yīng)助指數(shù) +1
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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樓2025-07-08 23:02:09
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