Today, plant fibers are considered as an important new renewable resource that can compete with some synthetic fibers, such as glass, in fiber-reinforced composites. In previous works, it was noted that the pectin-enriched middle lamella (ML) is a weak point in the fiber bundles for plant fiber-reinforced composites. ML is strongly bonded to the primary walls of the cells to form a complex layer called the compound middle lamella (CML). In a composite, cracks preferentially propagate along and through this layer when a mechanical loading is applied. In this work, middle lamellae of several plant fibers of different origin (flax, hemp, jute, kenaf, nettle, and date palm leaf sheath), among the most used for composite reinforcement, are investigated by atomic force microscopy (AFM). The peak-force quantitative nanomechanical property mapping (PF-QNM) mode is used in order to estimate the indentation modulus of this layer. AFM PF-QNM confirmed its potential and suitability to mechanically characterize and compare the stiffness of small areas at the micro and nanoscale level, such as plant cell walls and middle lamellae. Our results suggest that the mean indentation modulus of ML is in the range from 6 GPa (date palm leaf sheath) to 16 GPa (hemp), depending on the plant considered. Moreover, local cell-wall layer architectures were finely evidenced and described.

Plant fibres and especially flax can be distinguished from most synthetic fibres by their intricate shape and intrinsic porosity called lumen, which is usually assumed to be tubular. However, the real shape appears more complex and thus might induce stress concentrations influencing the fibre performance. This study proposes a novel representation of flax fibre lumen and its variations along the fibre, an interpretation of its origin and effect on flax fibre tensile properties. This investigation was conducted at the crossroads of complementary characterization techniques: optical and scanning electron microscopy (SEM), high-resolution X-ray microtomography (µCT) and mechanical tests at the cell-wall and fibre scale by atomic force microscopy (AFM) in Peak-Force Quantitative Nano-Mechanical property mapping (PF-QNM) mode and micromechanical tensile testing. Converging results highlight the difficulty of drawing a single geometric reference for the lumen. AFM and optical microscopy depict central cavities of different sizes and shapes. Porosity contents, varying from 0.4 to 7.2%, are estimated by high-resolution µCT. Furthermore, variations of lumen size are reported along the fibres. This intricate lumen shape might originate from the cell wall thickening and cell death but particular attention should also be paid to the effects of post mortem processes such as drying, retting and mechanical extraction of the fibre as well as sample preparation. Finally, SEM observation following tensile testing demonstrates the combined effect of geometrical inhomogeneities such as defects and intricate lumen porosity to drive the failure of the fibre.

PLA-flax non-woven composites are promising materials, coupling high performance and possible degradation at their end of life. To explore their ageing mechanisms during garden composting, microstructural investigations were carried out through scanning electron microscopy (SEM) and atomic force microscopy (AFM). We observe that flax fibres preferentially degrade ‘inwards’ from the edge to the core of the composite. In addition, progressive erosion of the cell walls occurs within the fibres themselves, ‘outwards’ from the central lumen to the periphery primary wall. This preferential degradation is reflected in the decrease in indentation modulus from around 23 GPa for fibres located in the preserved core of the composite to 3–4 GPa for the remaining outer-most cell wall crowns located at the edge of the sample that is in contact with the compost. Ageing of the PLA matrix is less drastic with a relatively stable indentation modulus. Nevertheless, a change in the PLA morphology, a significant decrease in its roughness and increase of porosity, can be observed towards the edge of the sample, in comparison to the core. This work highlights the important role of intrinsic fibre porosity, called lumen, which is suspected to be a major variable of the compost ageing process, providing pathways of entry for moisture and microorganisms that are involved in cell wall degradation.