Preparation of Polypropylene Fiber/Banana Fiber Composites by Novel Commingling Method

Sherely Annie Paul,1 Kuruvilla Joseph,2 Gem Mathew,3 Laly A. Pothen,1 Sabu Thomas4 1 Department of Chemistry, Bishop Moore College, Mavelikara, Kerala, India
2

Department of Chemistry, Indian Institute of Space Science and Technology, ISRO P.O, Thiruvananthapuram, Kerala, India Department of Chemistry, St. Thomas College, Pala, Kerala, India School of Chemical Sciences, Mahatma Gandhi University, Priyadharshini Hills P.O, Kottayam, Kerala, India

Short natural ber thermoplastic composites are usually fabricated by melt mixing or solution mixing followed by conventional methods like injection molding or compression molding. In melt mixing, the bers are subjected to high shear and this damage the natural ber. In solution mixing, the use of the organic solvent is essential and its use is hazardous. Development of a novel method commingling to prepare polypropylene (PP)/short natural ber composite is the main objective of this study. The inuence of ber loading on the mechanical properties of the composites prepared by the above method has been evaluated. The applications and limitations of several equations to predict physical properties such as tensile strength and modulus of the composites have been described. POLYM. COMPOS.,
31:816824, 2010. 2009 Society of Plastics Engineers

INTRODUCTION The interest in natural ber reinforced polymer composite is rapidly growing both in terms of industrial applications and basic research. The availability, renewability, biodegradability, low density, low cost and satisfactory mechanical properties of the natural bers make them an attractive ecological alternative to glass, carbon and man-made bers used for the manufacturing of composites [13]. High performance thermoplastic/natural ber composite materials offer signicant potential advantages than thermosets including higher damage tolerance, unlimited shelf life, faster component manufacturing time and greater recyclability. The main attraction of
Correspondence to: S. Thomas; e-mail: sabut552001@yahoo.com DOI 10.1002/pc.20864 Published online in Wiley InterScience (www.interscience.wiley.com). C V 2009 Society of Plastics Engineers

thermoplastic composite materials lies in the possibility of achieving very short remolding times as no chemical reaction is required. Because of the high viscosity of the thermoplastic matrix material, it is generally not easy to properly impregnate a ber reinforcement lay up during the manufacturing process. Due to these difculties in resin impregnation, intermediate materials that are partially impregnated have been developed which offer a route to more efcient manufacturing of thermoplastic composites [4, 5]. In general, the processing of thermoplastic composites is classied into two categories: pre-impregnation and post impregnation. In the former case, the bers are wetted and impregnated by the polymer in one step. The preimpregnated bers can be prepared by solution mixing or melt mixing. In post-impregnation, the polymers are available in the forms of lm, laments, or powder [6]. The bers and the polymer are mixed in a desired manner without any adhesion or bonding. Impregnation takes place during part fabrication. The polymeric bers can also be mixed with reinforcing bers to form a commingled bundle, which can be used in various applications. With commingling a good blending of matrix and reinforcement bers is possible [6]. R. Alagirusamy [7] studied the effect of the commingling process variables, namely air pressure and volume fraction of the matrix forming bers on the structure and properties of Glass/polypropylene, Glass polyester and Glass nylon commingled yarns. Dubouloz-Monnet et al. [8] reported the viscoelastic behavior of commingled composites of polypropylene reinforced by 22, 35, and 50 vol% of unidirectional glass bers, by taking into account qualitative and quantitative morphological analysis. The aim was to separate the mechanical properties of

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the different phases in order to reveal the presence of either an interphase or changes in PP chain motions due to the ber aggregates. Huang and Liu [9] investigated the properties of thermoplastic composites reinforced by ax fabrics. Flax yarn and PP (polypropylene) laments were twisted together to form a commingled yarn in a fancy twister. Fabrics with plain and twill weaves were woven by using the plied yarn. Composites with ve layers of identical fabric weaves were fabricated in a heating press. They analyzed the failure mechanism of the composite and structure of the broken end of the composites was observed by SEM (Scanning electron microscope). Tufail [10] reported the major problem observed during the use of a commingled material. i.e, de-commingling, wherein, the uniform distribution of ber and thermoplastic yarn gets disturbed which affects the nal quality of the composite. In the case of short natural ber reinforced thermoplastic composites, most of the samples are fabricated by preimpregnation method, i.e, melt mixing or solution mixing followed by conventional methods like injection molding or compression molding using thermoplastic granules [11]. In melt mixing, the bers are subjected to high shear and this damage the natural ber. In solution mixing, the use of the organic solvent like toluene/xylene is essential and its use is hazardous. Moreover it is very difcult to incorporate bers above 40% in melt mixing and in solution mixing. In the present article, we report the fabrication of the PP/banana ber composites by novel commingling method. In commingling, the polymer ber and reinforcement ber are intermingled together. Heating and consolidation of the commingled bers involve the melting of the dispersed polymer bers and the subsequent formation of a continuous polymer matrix around the reinforcement bers. In the present work we used short PP bers and short banana bers. During compression molding, the polypropylene bers melt and diffuse into the banana bers. Thus, polypropylene act as the matrix and banana ber act as the reinforcement. The advantage of this method is that reinforcement bers are not subjected to shear forces as in melt mixing. No solvents are required for mixing the polymer with reinforcement ber. Moreover percentage loading of the reinforcing bers could be increased up to 60%. Literature survey shows that very limited studies have been reported on natural ber composites prepared by using PP ber [1215]. No studies have reported in literature using commingling method for the preparation of short natural ber/PP ber composites. The elastic properties of short ber composites can be experimentally determined or derived from a variety of mathematical models. The advantage of a comprehensive mathematical model is that it reduces costly and time-consuming experiments. The variation of the amount of bers in a natural ber composite can be successfully chosen to correlate with the mechanical properties of composite. The amount of ber is one of the most important factors of any composite material since their mechanical properties are
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strongly dependent on it. The volume fraction of ber is commonly used to estimate certain mechanical properties of the composite material. The mechanical properties of a composite material depend primarily on the strength and modulus of the ber, the strength and the chemical stability of the matrix and the effectiveness of the bonding between matrix and ber in transferring stress across the interface [16]. In this article, the modied rule of mixtures, parallel, series and Halpin-Tsai models are applied to PP/ banana ber composites in order to compare the experimental results with the theoretical predictions MATERIALS AND METHODS Materials Polypropylene bers used as the polymer matrix with denier 900, % elongation 26, tenacity 4.53 g/d, weight average molecular mass 6.3 3 105 g/mol, density 0.91 were obtained from Gare Ware Ropes, India. Banana bers were obtained from Sheeba bers, Poovencode, Tamil Nadu. The banana ber was dried in an air oven at 708C for 6 h after chopping into 6-mm length for the preparation of the composites. The physical, mechanical properties and chemical constituents of the banana ber are reported in Table 1 [17]. Preparation of PP/Banana Fiber Composites Banana bers and PP bers were cut into 6- and 1-mm length, respectively. Fibers were mixed thoroughly and arranged in a tray measuring 150 3 150 3 3 mm3 and pressed into a mat. Short randomly oriented ber composite sheets were prepared by compression molding of the above mats at 170 6 38C and a pressure of 8 kg/cm2 for 3 min. The specimens were removed after cooling the mould at room temperature. PP/banana ber composites with different weight percentage of the bers were prepared in a similar manner. The schematic representation of the preparation of the commingled composite is given in Fig. 1. Mechanical Properties Measurement The tensile properties of composites were measured using a Universal Tensile Testing Machine at a crosshead
TABLE 1. Mechanical properties, chemical constituents and physical properties of banana ber. Properties Tensile strength (MPa) Tensile Modulus (GPa) Elongation at break (%) Cellulose content (%) Lignin content (%) Diameter of the ber (microns) Density (g/cm3) Banana ber 600750 2.93.2 24 6364 5 100125 1.3

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FIG. 1. The schematic representation of the preparation of the commingled composite.

FIG. 2. Stressstrain curve of PP/banana ber commingled composite with different banana ber loading:(1) Neat PP, (2) 10%, (3) 20%, (4) 30%, (5) 40%, (6) 50%, and (7) 60%.

speed of 50 mm/min and a gauge length of 50 mm. The test specimens were rectangular in shape with dimensions 120 3 15 3 3 mm3. The load-deformation curve was plotted to analyze the stress-strain behavior of the composites. Youngs modulus and elongation at break of the composites was determined from the stress strain curve. The three point exural properties were determined by the same machine according to ASTM D790. Charpy impact strength (unnotched) was measured in a WinPEN CEAST S. p. A. Italy according to ISO 179. The specimens dimension were 100 3 10 3 40 mm3. The impact energy was 2 Joules, impact velocity 2.9 m/s and the dissipation energy was 0.016 J. Hardness Hardness of the composites was measured using Shore D durometer. Optical Microscopy Olympus Magnus MSZ stereo microscope was used for observing the impact fracture surface of PP and PP/banana ber composites. RESULTS AND DISCUSSION Tensile Properties Effect of Fiber Loading. Figure 2 shows the stressstrain behavior of PP/banana ber composite at different ber loading. The behavior of neat PP is also presented in this gure. From the stress-strain curves, it can be seen that neat PP is more ductile and ductility decreases with the addition of bers. The stress is found to increase linearly with strain at low elongation for the
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composites. A decrease in slope at the second stage of the curve corresponds to the plastic deformation of matrix and to micro-crack initiation in the matrix. Thus gradual debonding of the bers from the matrix occurs during plastic deformation. The stress value is found to be higher for 50% ber composites and the value then decreases for 60% ber composites emphasizing the maximum allowable ber loading. Figures 3 and 4 show the effect of ber loading on the tensile strength and tensile modulus of the PP/banana ber composites. The tensile strength and modulus is found maximum when the ber loading is 50%. This is due to the reinforcement imparted by the bers which allows stress transfer from the matrix to the bers. At lower ber loading, the matrix is not restrained by enough bers and highly localized strains occur in the matrix at low stresses. As the ber loading increases up to 50%,

FIG. 3. Effect of banana ber loading on the tensile strength of PP/banana ber commingled composite.

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FIG. 4. Effect of banana ber loading on the tensile modulus of PP/banana ber commingled composite.

FIG. 5. Effect of banana ber loading on the elongation at break of PP/banana ber commingled composite.

the stress is more evenly distributed and the stiffness of the composite increases. It is observed that with the increase of ber loading from 10 to 50%, the tensile strength and tensile modulus of the composites increases to 42.65 and 38%, respectively. The composites containing 60% ber loading shows a decrease in tensile properties. The deviation at higher ber loading may be due to the ber packing and insufciently rich polymer regions. More over the possibility of ber entanglements and agglomeration results in the composite which leads to decrease in stress transfer between the matrix and the ber. If the matrix is insufciently available, the bers were no longer completely surrounded by the matrix at higher ber loading and voids are produced in the composite. It has been reported that most of the properties of the composites are affected by the presence of voids [18]. Houshyar et al. [18] calculated the void content of the PP/poly(propylene-co-ethylene) (PPE) composite with 10 60% ber loading and reported that 1030% samples has voids $0. On the other hand 60% sample has a void content of 19.3%. Elongation at break values of the composites as function of ber loading is shown in Fig. 5. It can be revealed from the gure that elongation at break decreases with increase in ber loading. This can be attributed to the fact that the reinforcing bers strongly restrain the deformation of the matrix polymer as demonstrated in several previous studies [19]. Flexural Properties Flexural strength is the measure of how well a material resists bending or what is the stiffness of the material. Unlike tensile loading, in exural testing all force is applied in one direction. The stresses induced due to the exural load are combination of compressive and tensile stresses. By the application of exural force, the upper and lower surface of the specimen under three point bendDOI 10.1002/pc

ing load is subjected to compression and tension and the axi-symmetric plane is subjected to shear stress. This creates two failure modes in the materials; bending and shear failure. The specimen fails when bending or shear stress reaches the corresponding critical value. A schematic representation of exural force acting on the specimen is given in Fig. 6. Figures 7 and 8 shows the effect of ber loading on the exural strength and exural modulus of PP/banana ber composites. From the gure it is clear that exural strength and modulus increases with ber loading and is maximum for 50% ber loading and then decreases due to the entanglement of the bers at higher loading as well as due to the ineffective wetting of the bers by the polymer. Thus the incorporation of banana bers (50%) into the PP matrix gave rise to a progressive increase of the exural strength from 36 to 56 MPa and exural modulus from 1.29 to 1.51 GPa. The improvement in tensile and exural properties is low below the critical ber loading because the reinforcing effect of the ber is not so good. Above the critical ber loading there is ber/ber entanglements which lead to a decrease of properties. Here the critical ber loading is found to be 50%. So the properties of the composites are found to be maximum at 50% ber loading. The improvement in properties will be less below and above the critical ber loading.

FIG. 6. Schematic representation of exural force acting on the specimen.

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FIG. 7. Effect of banana ber loading on the exural strength of PP/banana ber composite.

FIG. 8. Effect of banana ber loading on the exural modulus PP/banana ber composite.

The tensile and exural strength of the commingled composites were compared with that of composites prepared by solution mixing method. It was found that composites prepared by commingling method exhibited better mechanical properties when compared to the composites prepared by solution mixing method (Table 2).

Impact Behavior The impact strength becomes very important because cracks due to sudden loads are very common in service conditions. Forces (loads) of impact are applied so quickly that the relaxation of the molecular structure does not follow the process, resulting in fracture which can involve chain breaking and or interface separation. The impact strength of a composite depends upon many factors like toughness properties of the reinforcement, the nature of the interfacial region, geometry of the composite and test conditions. The nature of the interface region is of extreme importance in determining the toughness of the composite. If the interfacial bonding of the composite is weak, the crack will be propagated along the ber matrix/interface causing debonding. As a result of debonding, new surfaces will be produced which leads to a signicant increase in the energy absorbing capacity of the composites. In the case of short ber reinforced thermoplastic composites, the fracture is controlled by ber pullout. Cracks are found to form at the ber ends and misaligned bers are pulled through the matrix along with some ber fracture. In the case of short ber reinforced composites, ber length is also found to be an important parameter in controlling the impact strength, and the best results are obtained with bers having critical ber length. Inter laminar shear strength also affects the impact strength and increases with increasing shear strength. Impact strength can be improved by a number of ways [20] (a) by using intrinsically tough matrices, (b) by the application of a soft coating to the bers that will act as
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an interlayer after the composite is fabricated, (c) by using a weak interface between ber and the matrix. The Fig. 9 shows the impact strength of PP and PP/banana ber composites at different ber loading. The impact strength of the composite is higher than that of PP and found to increase with increase in ber loading upto 50% and then decreases. Cabral et al. [21] investigated the tensile and impact properties of jute-polypropylene composites as a function of the ber content. They found that tensile and impact strength sharply decreased after a critical ber volume fraction. They interpreted this change in the mechanical properties in terms of a change in the ber dispersion homogeneity, as well as of the interber contacts and the formation of interconnected paths within the thermoplastic matrix. Li et al. [22] studied the impact fracture toughness of saw dust/recycled PP composites. They observed that under impact loads, neat PP and the composites exhibited completely brittle behavior characterized by an abrupt decrease of load to zero after the maximum value. In the case of short ber reinforced polymers with ductile matrices, such as polypropylene, the major source of toughness derives from the matrix related energy mechanisms such as matrix shear deformation. The detrimental effect of the incorporation of natural bers to polypropylene on the impact fracture properties can be explained by the combined effect of the matrix embrittlement that occurs under the impact load and the restriction to matrix yielding imposed by the natural
TABLE 2. Comparison of tensile strength (T.S) and exural strength (F.S) of composites prepared by solution mixing method and commingling method. Banana ber loading (%) 10 20 30 Solution mixing method T.S (MPa) 18.0 21.0 24.0 F.S (MPa) 38.0 42.0 45.0 Commingling method T.S (MPa) 22.0 24.0 27.5 F.S (MPa) 42.0 45.0 48.0

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are carried out at room temperature, according to ABNT. Shore D durometer is used to measure the hardness of plastic composites. Results from Table 3 show that there is a decrease of hardness due to the introduction of bers. These results indicate that the presence of bers decreases the mechanical resistance to the penetration of another body or it can be a consequence of ber hygroscopicity, because water would have a plasticizing effect on the surface.

FIG. 9. Effect of banana ber loading on the impact strength of PP/banana ber composite.

bers. In addition, the interfacial adhesion also inuences the material fracture behavior. If a relatively weak interfacial bonding exists, ber/matrix debonding will induce local shear yielding of the PP matrix and the subsequent increase of toughness. In contrast if ber matrix debonding is suppressed as a result of an excessively strong interface, brittle fracture will occur and toughness will not be improved. Figure 10 shows a photomicrograph of fractured surface of PP/banana ber composite which suffered the mechanism of ber bridging due to the pendulum impact. The unnotched impact test specimens show visibly distinct modes in their fractured portions. The neat PP samples break clearly. In the case of PP/banana ber composite the ber breaks and comes out of matrix. It can be also seen that not all the bers of a composite are fractured during the impact test. A part of them develops a type of bridge between the two parts of the fractured matrix. As the crack spreads under the action of the applied load, a part of the load is transferred to the bers which are elastically deformed [23].

Hardness of the Composites Hardness provides information about material tenacity or fragility, because it is related to the module and mechanical resistance of the material to the penetration of a body [24]. In all the methods of hardness testing the thickness of the material and the nature of substrate are very important, because the elasticity is usually also measured. It should be noted that hardness tests always measure the hardness of the surface and not the inner part of the material. The hardness property must still be evaluated with caution, because the surface layers of the polymers can present different molecular orientations, levels of residual tension and other different properties when compared to the whole material [24]. Shore hardness tests
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FIG. 10. Digital photomicrograph of the fractured surface of (a) neat PP (b) PP/banana ber composite, (c) Magnied view of b (Magnication 3150). [Color gure can be viewed in the online issue, which is available at www.interscience.wiley.com.]

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TABLE 3. Hardness of PP/banana ber commingled composite. Material PP PP/10% PP/30% PP/50% PP/60% Hardness 72 70 65 62 55

banana banana banana banana

ber ber ber ber

where Tc, Tm, Tf are the tensile strength of the composite, matrix and ber respectively. If modulus is the parameter under study, notations such as Mc, Mm and Mf may be used instead of Tc, Tm, and Tf where Mc, Mm, and Mf are the Youngs moduli of composite, matrix and ber, respectively. Hirsch Model. Hirsch Model [31] is a combination of Parallel and Series models. The schematic representation of Hirsch Model is shown in Fig. 11 [32]. Using this model, the tensile strength and Youngs modulus are determined by the equations Tc xTm Vm Tf Vf 1 x Tm Tf T m V f Tf V m 5

Theoretical Modeling In the literature, several theories and equations have been developed to model the relation between the tensile properties of the composite and the parameters such as ber length, ber orientation, ber dispersion, ber geometry and the degree of interfacial adhesion between the ber and the matrix [2528]. These are (1) Modied rule of Mixtures, (2) Series model, (3) Parallel model, (4) Hirsch model, and (5) HalpinTsai model. Modied Rule of Mixtures. The modied rule of mixtures [29] can be given as follows. Tc Tm 1 Vf Tf Vfe 1

where v is a parameter which determines the stress transfer between the ber and the Matrix. In terms of the modulus, the equation is Mc xMm Vm Mf Vf 1 x Mm Mf M m Vf M f Vm 6

where Tc is the ultimate strength of the composites, Tm is the matrix strength at the failure strain of the ber, Tf is the ultimate strength of ber, Vf is the ber volume fraction and Vfe is the effective ber volume fraction. The effective ber volume fraction is given in terms of the ber volume fraction and the ratio of real contribution as follows Vfe Vf 1 P; where P is the degradation parameter for the effective ber volume fraction, lying between 0 and 1. P can be calculated from the micro geometry of the composite components and depends only on the ber volume fraction because the micro geometry is intimately related to the ber volume fraction under identical manufacturing conditions. P can be calculated from the equation P DTc Tf Vf 2

HalpinTsai Model. Several researchers used Halpin Tsai model [33] to determine the properties of the composites that contain discontinuous bers oriented in the loading direction. The tensile strength can be calculated using the model as follows Mc xMm Vm Mf Vf 1 x Mm Mf M m Vf M f Vm 7

where DTc is the difference between the experimentally measured strength and the strength predicted by the rule of mixtures. Parallel and Series Models. The parallel and series models [30] are used to determine the modulus and tensile strength of short ber composites. The equations for tensile strength are Tc Tf Vf Tm Vm Parallel model Tc Tm Tf Series model Tm Vf Tf Vm 3 4

FIG. 11. A schematic representation of Hirsch Model.

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8 9 > 1 AgVf > > Tc Tm > : ; 1 gWVf where Tf =Tm 1 Tf =Tm A 9 8 >1 /max > >V > > f W1> ; : /2 max g

9 10

where is umax is the packing fraction of the bers. The value of packing fraction for different ber arrangement in the matrix has already reported in the literature [19]. The different arrangements of bers in the matrix include square packing, hexagonal packing and random packing. In the present case, it is assumed that the bers are randomly close packed in the matrix. Therefore the value of umax is 0.82 is substituted in the Eq. 10. The experimental and theoretical values of tensile strength of the composite as a function of ber loading (10, 20, and 30%) of the composites are given in the Fig. 12. It can be seen that, in all cases, tensile strength increases regularly with increase in ber loading. A good correlation between the theoretically and experimentally observed tensile strength was seen in model predicted by the modied rule of mixtures. The experimental value exactly ts with the theoretical value in the case of this model. This model predicts the actual composite strength because the value of q is dened to account for the microgeometry of real composites. Series Model and Halpin Tsai Model show some what agreement with the experimental value. But the parallel and Hirsch Models agree the least with the experimental values. It can be seen from Fig. 12 that at lower ber loading, Parallel and Hirsch Model show more agreement with experimental values. This can be attributed to the fact that at lower

FIG. 13. The experimental and theoretical value of tensile modulus of the composites as a function of banana ber loading.

ber loading, uniform stress or strain in the composite is achieved as a result of better distribution of load through the well-dispersed bers in the matrix. But at higher ber loading, some of the bers will be agglomerated in the matrix. Hence the applied load will be distributed unevenly between non-aggregated and aggregated bers. The Youngs modulus value of the composite samples (10, 20, and 30%) is compared with the theoretical predictions in Fig. 13. Series model is in good agreement with the experimental value. Hirsch model (X 0.2) shows slight positive deviation. But parallel models show still large positive deviation from the experimental value. It was also found that better agreement between the theoretical and experimental modulus values is observed at lower ber loading when compared to higher ber loading. The limitations of the models used in the study mainly depend on different factors. The chance of the formation of microvoids between the ber and the matrix during the preparation of the composites greatly inuence the tensile properties of the composites. The number of voids increases with increase in ber loading. This factor is not accounted for any of the models used in this study. The presence of voids, ber-ber interaction, and critical ber length, non-uniformity of the ber and the surface irregularities of the ber may be the other reasons. More over natural bers cant be produced with a denite range of properties like glass ber. Their characteristics properties like tensile strength and modulus may vary considerably from ber to ber.

CONCLUSIONS In this article, novel commingling method is introduced for the preparation of short natural ber polypropylene composites. Advantage of commingling method is that it is environmentally benign. Tensile properties of the above composites were studied as a function of ber
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FIG. 12. The experimental and theoretical value of tensile strength of composites as a function of banana ber loading.

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loading. It was found that tensile properties of the composite increased with ber loading up to 50%. It was also observed that hardness of PP is decreased by the introduction of bers and it decreased with the increase in ber loading. The experimental results of the tensile properties of the composites were compared with the theoretical prediction. The best correlation between the theoretically and experimentally observed tensile strength was seen in model predicted by the modied rule of mixtures. REFERENCES
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