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

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solution (pH 4) for 4 h at 85°C. Lignin was oxidized and extracted in chlorite solution<br />

for 1 h at 75°C (300 ml water+10 g NaClO2+1 ml 100% acetic acid). Hemicellulose was<br />

extracted in 100 ml 12% NaOH+2% H3BO3 solution for 90 minutes at 25°C. After each<br />

step the suspension was filtrated on pre-weighed glass filters and the filter cake washed<br />

in water. The contents were determined from the dry matter loss in the extraction steps<br />

by drying overnight at 60°C and weighing after each step. The mineral content was<br />

determined by incineration <strong>of</strong> 1 g raw sample at 550°C for 3 h.<br />

Tensile tests on <strong>fibre</strong> bundles (15 mm long lf) were done with a 3 mm test span lspan at a<br />

strain rate <strong>of</strong> 1.7×10 -3 s -1 using an Instron 5566 with pressley clamps [Type: Stelometer<br />

654 from Zellweger Uster] (Thygesen et al., 2005a). Following fracture the <strong>fibre</strong> pieces<br />

<strong>of</strong> 15 mm were weighed wf. The number <strong>of</strong> repetitions was at least 13 for each sample.<br />

The failure stress σfu was calculated based on the failure force Ffu and the <strong>fibre</strong> density<br />

ρf:<br />

σ<br />

F l × ρ<br />

fu<br />

f f<br />

fu = = Ffu<br />

×<br />

Equation 1<br />

Af<br />

w f<br />

The <strong>fibre</strong> density for the investigated <strong>hemp</strong> <strong>fibre</strong>s and <strong>hemp</strong> yarn is 1.58 g/cm 3 (Madsen<br />

2004; Thygesen 2006). The maximum density for pure and fully crystalline cellulose is<br />

in the range 1.61 to 1.64 g/cm 3 , based on crystallographic information (Nishiyama et al.,<br />

2002; Thygesen et al., 2005b).<br />

Preparation <strong>of</strong> <strong>composites</strong><br />

The <strong>fibre</strong> bundles <strong>of</strong> 6 – 25 cm length were wetted in water and aligned by carting with a<br />

comb. In cases <strong>of</strong> short <strong>fibre</strong> pieces (6 cm), the aligned <strong>fibre</strong>s were placed on top <strong>of</strong> each<br />

other in three layers with different <strong>fibre</strong>-end positions to allow stress transfer between<br />

the <strong>fibre</strong>s and reduce movement <strong>of</strong> the <strong>fibre</strong>s in the epoxy flow when the lay-up was<br />

being compressed. The <strong>hemp</strong> yarn <strong>composites</strong> were made both by hand carting and<br />

filament winding (Madsen & Lilholt, 2003). The <strong>fibre</strong> content in the <strong>composites</strong> was<br />

controlled by the displacement rate during winding. The frame was displaced at a rate<br />

that allowed 11 rotations/cm. The epoxy resin (SPX 6872) and hardener (SPX 6873)<br />

were mixed in a ratio <strong>of</strong> 100 g resin to 36 g hardener and poured over the <strong>fibre</strong>s and left<br />

for 5 – 10 minutes to allow impregnation. Spacers <strong>of</strong> 1.5 mm thickness were used to<br />

control the laminate thickness. Tape was placed beside the <strong>fibre</strong>s to avoid <strong>fibre</strong><br />

movement. Finally, a steel plate was placed on the mould and excess resin with air<br />

bubbles was squeezed out with clamps. The lay-up was pre-cured at 40°C for 16 hours<br />

and thereafter cured at 120°C for 6 hours.<br />

<strong>An</strong>alysis <strong>of</strong> the <strong>composites</strong><br />

Standard dumb-bell-shaped tensile test specimens (180 × 20 mm with gauge section <strong>of</strong><br />

25 × 15 mm) were cut from the laminates. Tensile tests were performed at room<br />

temperature on an Instron machine with crosshead speed <strong>of</strong> 1 mm/min. The strain was<br />

measured with two extensometers placed on each side <strong>of</strong> the test specimens.<br />

Composite structure and <strong>fibre</strong> bundle size were investigated by SEM-microscopy.<br />

Composite pieces were polished on the side perpendicular to the <strong>fibre</strong> direction using<br />

wetted silicon carbide paper [Struers, Denmark] in a series <strong>of</strong> decreasing roughness<br />

Risø-PhD-11 125

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