Three types of plant fibers are used in this work: Triumfetta cordifolia bast fibers collected in Cameroon and extracted by water retting according to the method used in the literature Mewoli et al. [15] and cut by a cutter set to a length of 120mm; flax fibers (Linum usitatissimum L.) are provided by CALIRA (France) and hemp fibers supplied by GEOChanvre (France). These different fibers are used as reinforcement in the nonwoven with polylactide fibers (PLA INGEO™ Biopolymer type SLN 2660D) as matrix. They are supplied by PERVIRA cooperative (Germany), they have an average length of 64 mm, an average diameter of 6 Dtex and a density of 1.24 g/cm3. Table 1 shows the properties of the plant fibers, non-woven felts.
2.2. Manufacture of non-woven biocomposites
The manufacturing process of the biocomposites is illustrated in Fig. 1. First, using the carding-napping-needling technology of CETELOR (Epinal, France), the needle-punched nonwoven structures were elaborated from the mixture of PLA/TC, PLA/flax and PLA/hemp fibers. The vegetable fibers and the thermoplastic polymer fibers of PLA are introduced in a ratio weight of reinforcement/matrix of 50:50 in the Laroche opening machine at a speed of 1800 rpm, where they are individualized and mixed in order to be conveyed in a loader and then in the carding machine of Bonino brand which makes it possible to obtain homogeneous webs. These undergo at the exit of the carding machine, a topping where they are piled up to form a web of webs of a certain mass density followed by a consolidation by needling of 150 blows/cm2, which leads to the non-woven structure. It should be noted that the orientation of the needle-punched web is close to a 90° angle with respect to the machine direction (MD) of the reinforcing roll.
In a second step, the biocomposites are shaped by thermocompression, on a branded hydraulic press (LabTech Scientific 50T) at EcoTechnilin SAS (Normandy, France) from superimposed nonwoven felts to reach a mass per unit area of 1500 ± 50 g/m², then hot-pressed at 200°C and 40 bars for 180 seconds before being cooled down at 50 bars for an additional 40 seconds to obtain rigid sheets of 250 x 200 mm² dimensions. Two thicknesses (2 and 3 mm) were fixed by the use of wedges.
2.3. Measurement of density, fiber density fraction and porosity rate
To calculate the constituents of the nonwoven, the dichloromethane (DCM) resin digestion method (PLA) in accordance with the literatures of Alimuzzaman, [29] and Akonda et al. [30] was used. The anhydrous mass of the sample was determined before and after matrix digestion. Non-woven felt (PLA/plant fiber) specimens were soaked in a bath containing 100ml DCM at room temperature to digest the matrix. Sintered glass crucibles, oven, desiccants, DCM, conical flasks, and a balance were used in this experiment. For these experiments, the average values were calculated from four measurements and considered as the final value. The fiber content, void content, and volume fraction of plant fibers were calculated using the following equations (1)–(6):
\({W}_{f}\left(\%\right)=\)\(\frac{{m}_{3}-{m}_{1}}{{{m}_{2}-m}_{1}}\times 100\) (1)
Where, \({W}_{f}\) is the fiber content as a percentage of the initial mass; m1 is the sintered glass crucible (g); m2 is the initial mass of the sample and glass crucible (g); m3 is the final total mass (g) of crucible and residue after digestion.
\({W}_{r}\left(\%\right)=\)\(100-{P}_{f}\) (2)
To measure the density of the biocomposite, the calculation was based on the assumption that the mass of the final plate is the sum of the mass of the fibers (reinforcements) and the resin. The total volume of the biocomposite was realized with the measurements of the plate dimensions (\({V}_{c }\)= \(L\times l\times t\)). \({V}_{c}\): total volume of biocomposite in (m3); \(L\): length of biocomposite plate in (mm); \(l\): width of biocomposite plate in mm; \(t\): thickness of biocomposite plate in (mm). The density of the biocomposite is given by Eq. (3):
$${\rho }_{c}=\frac{{m}_{c}}{{V}_{c}}$$
3
Where, \({\rho }_{c}\) is the density of the biocomposite \({m}_{c}\); is the mass of the biocomposite weighed in (g) and \({V}_{c}\) total calculated volume in m3.
$${V}_{f}={W}_{f}\times \frac{{\rho }_{c}}{{\rho }_{f}}$$
4
Where \({V}_{f}\)is the fiber content as a percentage of the initial volume, \({W}_{f}\) is the fiber content as a percentage of the initial mass, \({\rho }_{c}\) is the density of the test sample (g/m3), \({\rho }_{f}\) is the density of the flax, hemp and TC fibers (g/m3).
$${V}_{r}=(100-{W}_{f})\times \frac{{\rho }_{c}}{{\rho }_{f}}$$
5
Where, \({V}_{r}\)is the PLA content as a percentage of the initial volume; \({W}_{f}\) is the fiber content as a percentage of the initial mass; \({\rho }_{c}\) is the density of the test sample (g/m3); \({\rho }_{r}\) is the density of PLA (g/m3).
The porosity rates are determined on the composite materials after thermocompression using equations (6).
$$ɸ =100\left[{W}_{f}\times \frac{{\rho }_{c}}{{\rho }_{f}} +\left(100-{W}_{f}\right)\times \frac{{\rho }_{c}}{{\rho }_{r}} \right]$$
6
Where, \(ɸ\) is the void content as a percentage of the initial volume, \({W}_{f}\) is the fiber content as a percentage of the initial mass, \({\rho }_{c}\) is the density of the specimen (g/m3), \({\rho }_{f}\) is the density of the flax, hemp and TC fibers (g/m3), \({\rho }_{r}\) is the density of PLA (g/m3).
2.4. Mechanical characterization of the biocomposite
The tensile and bending behavior of PLA biocomposite materials was studied in both directions of the reinforcement, MD (Machine Direction) and CD (Cross Direction) as well as the influence of the thickness of PLA biocomposites reinforced with TC, linen and hemp fibers.
2.4.1. Traction
Static tensile tests were performed on the materials using an INSTRON model 4206 testing machine equipped with a 100 kN load cell with a crosshead speed of 2mm/min and a nominal length of 150mm between the jaws. The tests were performed on specimens in a controlled atmosphere (23°C and 50% RH), according to the ISO 527-4 standard. The tensile modulus was calculated in the linear part of the stress-strain curve, at the beginning of the load between 0.05% and 0.1%.
2.4.2 Three-point bending
Three-point bending tests were performed in accordance with BS EN ISO 14125 to determine the bending behavior. Five specimens of each sample were tested on an INSTRON model 4301 with a 30 kN load cell at a crosshead speed of 2 mm/min. The deformation in the middle was given by the displacement of the center load element, and the specimen dimensions were 100 × 25 mm2 with a span ratio of 1:20. All tests were performed at a temperature of 23 ± 2°C and a relative humidity of 50 ± 5%. Modulus of elasticity in bending, \({E}_{f}\) was calculated in the linear part of the stress-strain curve, at the onset of loading between 0.05% and 0.25%.