Comparison of sample crystallinity determination methods by X-ray diffraction for challenging cellulose I materials
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- 作者：Patrik Ahvenainen ; Inkeri Kontro ; Kirsi Svedström
- 关键词：Cellulose ; Crystallinity ; X ; ray diffraction ; Wide ; angle X ; ray scattering
- 刊名：Cellulose
- 出版年：2016
- 出版时间：April 2016
- 年：2016
- 卷：23
- 期：2
- 页码：1073-1086
- 全文大小：1,572 KB
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Inkeri Kontro (1)
Kirsi Svedström (1)
1. Department of Physics, University of Helsinki, P.O. Box 64, 00014, Helsinki, Finland - 刊物类别：Chemistry and Materials Science
- 刊物主题：Chemistry
Bioorganic Chemistry
Physical Chemistry
Organic Chemistry
Polymer Sciences - 出版者：Springer Netherlands
- ISSN：1572-882X
文摘
Cellulose crystallinity assessment is important for optimizing the yield of cellulose products, such as bioethanol. X-ray diffraction is often used for this purpose for its perceived robustness and availability. In this work, the five most common analysis methods (the Segal peak height method and those based on peak fitting and/or amorphous standards) are critically reviewed and compared to two-dimensional Rietveld refinement. A larger (\(n=16\)) and more varied collection of samples than previous studies have presented is used. In particular, samples (\(n=6\)) with low crystallinity and small crystallite sizes are included. A good linear correlation (\(r^{2} \ge 0.90\)) between the five most common methods suggests that they agree on large-scale crystallinity differences between samples. For small crystallinity differences, however, correlation was not seen for samples that were from distinct sample sets. The least-squares fitting using an amorphous standard shows the smallest crystallite size dependence and this method combined with perpendicular transmission geometry also yielded values closest to independently obtained cellulose crystallinity values. On the other hand, these values are too low according to the Rietveld refinement. All analysis methods have weaknesses that should be considered when assessing differences in sample crystallinity.