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Properties of hemp fibre polymer composites -An optimisation of ...

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By TEM microscopy, the single fiber middle lamellae (ML) and primary wall (P) were<br />

found to have thickness <strong>of</strong> 30-50 nm and 70-110 nm, respectively (Figure 3A, B). The<br />

secondary cell wall was composed <strong>of</strong> a 100-130 nm thick S1 layer and a 3-13 μm thick<br />

S2 layer. Both SEM and TEM observations showed that the S2 layer had a laminate<br />

structure <strong>of</strong> 1 to 4 major concentric layers <strong>of</strong> 1-5 μm in thickness. The major layers were<br />

constructed <strong>of</strong> 100 nm thick lamellae (Figure 1C-D, Figure 3C). Thin layers <strong>of</strong> 200-240<br />

nm in thickness were located between the major concentric layers (Figure 3A).<br />

Confirmation for a concentric orientation <strong>of</strong> the layers was further obtained by SEM<br />

observations on the ends <strong>of</strong> P. radiata Cel 26 treated fibers fractured under tension<br />

(Figure 4). The major layers separated from each other, further indicating that they were<br />

weakly attached to one another.<br />

Micr<strong>of</strong>ibril angles <strong>of</strong> the single fibers<br />

Some single fibers in the H2O2 delignified <strong>hemp</strong> showed evidence <strong>of</strong> cavities made by<br />

naturally occurring fungi before harvest. It was possible to measure the micr<strong>of</strong>ibril angle<br />

in two adjacent cell wall layers since several parallel cavities crossed each other (Figure<br />

5A). The micr<strong>of</strong>ibrils had Z helical orientation with angles in the intervals 0-5° and 25-<br />

30°. Superficial attack <strong>of</strong> other single fibers showed evidence <strong>of</strong> MFAs in the range <strong>of</strong><br />

70-90° with an S helical orientation (Figure 5B), which was confirmed by polarized light<br />

microscopy (data not shown). Single fibers from H2O2 delignified and P. radiata Cel 26<br />

treated <strong>hemp</strong> stems showed regions where the S1 layer was partly peeled <strong>of</strong>f (Figure<br />

5C). The cellulose aggregates in the S1 and S2 layer beneath were orientated<br />

perpendicular and parallel to the fiber axis, respectively. The fracture experiments<br />

(Figure 4) showed evidence for a main S2 MFA <strong>of</strong> 0-10° agreeing with 4° measured<br />

previously by X-ray diffraction (Fink et al., 1999). The micr<strong>of</strong>ibril model <strong>of</strong> the single<br />

fibers shown in Figure 2B is based on the obtained data.<br />

Figure 4. Fractured end <strong>of</strong> a single fiber showed at increasing magnification. A: Splits<br />

developed by radial tension between the major concentric layers due to the weak<br />

interface. B: Cellulose aggregates (arrows) apparent at site <strong>of</strong> fracture.<br />

Risø-PhD-11 97

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