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<p>In this work, we propose an X-ray diffraction characterization of the flax ultrastructure to improve our understanding of its role in expressing the complex mechanical behaviour of flax fibres. Initially, X-ray diffraction measurements were performed on both undeformed and deformed samples consisting in fibre bundles and using for the first time, the combined “structure/microstructure/texture” analysis method implemented in the Maud software and based on a Rietveld algorithm. For all the fibre bundles, the microstructural analysis showed that these microfibrils, having a cellulose Iβ structure, exhibit an ellipsoidal&#xa0;crystallite shape elongated along their c-axis. The results also suggest the existence of a paracrystalline cellulose phase in the flax ultrastructure, with a degree of order intermediate between amorphous and crystalline Iβ cellulose. The corresponding quantitative texture analysis allowed to access the microfibril angle distribution in the flax secondary wall, with cellulose microfibrils inclined with respect to fibre axes with angles in the 0–20° range and a maximum of the distribution around 5°–10°. The combination of tensile tests and in-situ X-ray diffraction measurements put in evidence a substantial rearrangement of the microfibril angle distribution confirming the reorientation of cellulose microfibrils along the fibre axis. However, this evolution is non-linear and appears significant for deformations below 0.6%, becoming relatively weak or attenuated for higher deformations. This X-ray combined analysis provides new insights into the organization of cellulose in flax fibres, and by extension, plant fibres in general.</p>

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X-ray diffraction combined analysis method for the determination of cellulose crystal ultrastructure for free and deformed flax fibre bundles

  • 期刊论文

  • 发表日期：

    2025年11月19日

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  • Magali Morales,
  • Komlavi Gogoli,
  • Daniel Chateigner,
  • Luca Lutterotti,
  • Christophe Poilâne,
  • Florian Gehring,
  • Gregory Stoclet,
  • Olivier Perez

摘要

In this work, we propose an X-ray diffraction characterization of the flax ultrastructure to improve our understanding of its role in expressing the complex mechanical behaviour of flax fibres. Initially, X-ray diffraction measurements were performed on both undeformed and deformed samples consisting in fibre bundles and using for the first time, the combined “structure/microstructure/texture” analysis method implemented in the Maud software and based on a Rietveld algorithm. For all the fibre bundles, the microstructural analysis showed that these microfibrils, having a cellulose Iβ structure, exhibit an ellipsoidal crystallite shape elongated along their c-axis. The results also suggest the existence of a paracrystalline cellulose phase in the flax ultrastructure, with a degree of order intermediate between amorphous and crystalline Iβ cellulose. The corresponding quantitative texture analysis allowed to access the microfibril angle distribution in the flax secondary wall, with cellulose microfibrils inclined with respect to fibre axes with angles in the 0–20° range and a maximum of the distribution around 5°–10°. The combination of tensile tests and in-situ X-ray diffraction measurements put in evidence a substantial rearrangement of the microfibril angle distribution confirming the reorientation of cellulose microfibrils along the fibre axis. However, this evolution is non-linear and appears significant for deformations below 0.6%, becoming relatively weak or attenuated for higher deformations. This X-ray combined analysis provides new insights into the organization of cellulose in flax fibres, and by extension, plant fibres in general.