Metrological characterization of X-ray diffraction methods for determination of crystallite size in nano-scale materials
Metrological characterization of X-ray diffraction methods for determination of crystallite size in nano-scale materials
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DOI：
10.1016/j.matchar.2006.09.002
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发表时间：
2007-10
影响因子：
4.7
通讯作者：
V. Uvarov;I. Popov
中科院分区：
文献类型：
--
作者：
V. Uvarov;I. Popov
采用x射线衍射法测定了210种TiO2（锐钛矿）纳米晶粉体的晶粒尺寸，晶粒尺寸为3 ~ 35 nm。每个x射线衍射图都使用不同的免费和商业软件进行处理。采用Scherrer方程和Warren-Averbach方法计算晶体尺寸。对所得结果进行统计处理和比较评估，以确定所得差异的统计显著性。对于小于10 nm的晶体，使用Scherrer方程得到的结果的平均绝对差值不超过0.36 nm，在10 - 15 nm范围内为0.54 nm，在> - 15 nm范围内为2.4 nm。我们还发现，增加分析时间可以改善统计结果，但不影响计算出的晶粒尺寸。由x射线数据测定的晶体尺寸值与透射电子显微镜成像的值吻合得很好。
Crystallite size values were determined by X-ray diffraction methods for 210 TiO2(anatase) nanocrystalline powders with crystallite size from 3 nm to 35 nm. Each X-ray diffraction pattern was processed using different free and commercial software. The crystallite size calculations were performed using Scherrer equation and Warren–Averbach method. Statistical treatment and comparative assessment of the obtained results were performed for the purpose of an ascertainment of statistical significance of the obtained differences. The average absolute divergence between results obtained with using Scherrer equation does not exceed 0.36 nm for the crystallites smaller than 10 nm, 0.54 nm for the range 10–15 nm and 2.4 nm for the range >15 nm. We have also found that increasing the analysis time improves statistics, however does not affect the calculated crystallite sizes. The values of crystallite size determined from X-ray data were in good agreement with those obtained by imaging in a transmission electron microscope.