Composite Structures 197 (2018) 63–71

Contents lists available at ScienceDirect

Composite Structures
journal homepage: www.elsevier.com/locate/compstruct

Properties of flax-polypropylene composites made through hybrid yarn and T

film stacking methods
⁎
Mahadev Bar , R. Alagirusamy, Apurba Das
Department of Textile Technology, Indian Institute of Technology Delhi, New Delhi, India

A R T I C LE I N FO A B S T R A C T

Keywords: In the present study, two distinguishable unidirectional composite structures have been produced using com-
Bio-composites pression molding technique. Among these two, one is made through conventional film stacking (FSC) method
Natural fibre while the other structure is made after consolidating the DREF spun hybrid yarns (DYC). In both cases, low
Composite structure twisted, MAgPP treated flax yarns are used as reinforcement and polypropylene (PP) is used as matrix. Effects of
Mechanical properties
fibre content on both composite structures are studied at 40%, 50% and 60% flax contents respectively. It has
Hybrid yarn
been observed that irrespective of composite structure, the tensile and flexural properties of the composite
samples increase with increasing flax content but the impact strength decreases with increasing flax content.
However, at constant fibre volume fraction, the DYC composites demonstrate better properties than the FSC
composites. This is mainly due to better fibre-matrix distribution and lower void content of the DYC composites
than the FSC composites.

1. Introduction regarding poor fibre-matrix adhesion, poor thermal stability of natural

fibres etc. Researchers have addressed these problems and have
At present, the natural fibres and the thermoplastic polymers are achieved remarkable improvement in natural fibre composite proper-
drawing a substantial attention of the researchers and the resultant ties [15–17].
composites are finding huge applications in different consumer in- Then again, when it comes to natural fibre reinforced thermoplastic
dustries [1–3]. This can be broadly attributed to two factors. Firstly, composite a new problem arises regarding high melt viscosity of ther-
increase in environmental awareness and the matchless attributes of the moplastic resin. High melt viscosity causes uneven resin penetration in
natural fibres over the synthetic fibres [4,5]. Secondly, the advantages the fibrous preforms. The resin penetration into the reinforcing fibrous
of thermoplastic polymers over the thermoset and biodegradable preforms can be improved by applying high consolidation pressure but,
polymers [6,7]. Thermoset polymers are non-biodegradable and non- at the same time high consolidation pressure de-aligns the reinforcing
recyclable in nature which promote the problems associate with global fibres, apart from increasing the power consumption [18]. Insufficient
waste disposal and land fill of waste products [8]. However, the bio- resin penetration, uneven fibre-resin distribution and reinforcing fibre
degradable polymers do not promote the above mentioned problems de-alignment ultimately result in a composite with inferior mechanical
but the cost of the bio-degradable polymers is comparatively high and properties [19–21]. Keeping the above mentioned drawbacks and pre-
they have limited availability. Moreover, most of the bio-degradable dicted growing market size in mind, it is very much necessary to carry
polymers are brittle in nature and their mechanical and other perfor- out some fundamental studies on the fabrication process of natural fibre
mances still trail the conventional petroleum based engineering poly- reinforced thermoplastic composite.
mers [8,9]. Thermoplastic polymers are recyclable, ductile, easy to Natural fibre reinforced thermoplastic composites are fabricated
store, non-corrosive, have low density, long self-life (the time for which through different methods. Among these methods, compression
the material remain usable), shorter curing cycle, good mechanical molding is very popular for its high reproducibility, easy handling, low
properties; can overcome the short-comings of the thermoset polymers maintenance, capability of manufacturing complex geometry structures
[10–12]. In a recent survey, it is reported that with the introduction of etc. [22]. In compression molding, natural fibres are generally re-
thermoplastic polymer as matrix the market size of natural fibre com- inforced either in randomly distributed form or in the form of woven
posites is growing exponentially and it will reach to $5.83 billion by textile preforms. Random fibre orientation offers poor mechanical
2019 [13,14]. However, natural fibre composites have some limitations properties of the resultant composite and textile preform reinforcement

⁎
Corresponding author.
E-mail address: mahadevbar07@gmail.com (M. Bar).

https://doi.org/10.1016/j.compstruct.2018.04.078
Received 24 November 2017; Received in revised form 15 April 2018; Accepted 26 April 2018
Available online 27 April 2018
0263-8223/ © 2018 Elsevier Ltd. All rights reserved.
M. Bar et al. Composite Structures 197 (2018) 63–71

produces thermoplastic composite structure with voids, which are not content in both composite structures is varied between 40% and 60%.
desirable [19,20]. Finally, the effect of composite structures on different composite
Presently, hybrid yarns are in the center of attention of the com- properties such as tensile, flexural and impact properties have been
posite researchers. In the context of thermoplastic composite, hybrid studied.
yarns are the yarns having both the reinforcing and matrix forming
fibre components in its structure. Alagirusamy et al. [18] have sum- 2. Materials and methods
marized different types of hybrid yarn used for thermoplastic composite
manufacturing. It is observed that DREF (Dr. Ernst Fehrer AG, Austria) 2.1. Materials
spinning technique has few more advantages over all other existing
hybrid yarn manufacturing methods. For instance, DREF spinning offers PP, in both fibre or in film forms, having a density of 0.91 g/cm3,
very high rate of production with minimum damage or no damage to melting temperature of 165 °C and melt flow index 1 g/min (tested at
the core yarn. Hybrid yarns with wide range of core to sheath ratios can 190 °C temperature with 2.16 kg weight) are used as sheath or matrix
be manufactured using this method [23]. In some recent studies, re- component. Flax yarn having a linear density of 165 g/km and a twist of
searchers have developed natural fibre based hybrid yarn structures 28 turns per meter (TPM) is used as reinforcing component after un-
through different techniques such as commingling [24], braiding [25], twisting in ring spinning machine. PP was supplied by M/s Zenith Fibre
wrap spinning [26] etc. It has been observed that hybrid yarn improves Ltd., Gujarat, India and the flax yarn (having a twist of 320 TPM) was
the thermoplastic resin distribution in the composite structure by re- procured from M/s Jayashree Textile Ltd. West Bengal, India. Maleic
ducing effective resin flow distance. However, most of the studies on Anhydride grafted Polypropylene (MAgPP) having Maleic Anhydride
natural fibre based hybrid yarn reinforced thermoplastic composite are content between 1.6% and 2.5%; melt flow index 5 g/min is used as a
carried out using twisted core based hybrid yarn [24–26]. Yarn twist coupling agent. It was procured from Pluss polymers Pvt. Ltd., Gurgaon,
restricts the resin penetration into the yarn core and it ultimately results India.
in composite structure with voids. Twist also reduces the ultimate fibre
strength utilization to the final composite [19,27]. Zhang et al. [26] 2.2. DREF yarn preparation
have developed a flax-PP commingled wrap spun yarn in which all flax
fibres remain in a twist-less state. They have also studied the effec- The DREF or friction spinning system is an open end spinning pro-
tiveness of the commingled wrap spun yarn on the flexural properties of cess, was developed by Dr. Ernst Fehrer, in 1973. The DREF spinning
the resultant composites. It is observed that the wrap spun yarn sig- process can produce core-sheath structured hybrid yarn at very high
nificantly enhances the flexural strength and modulus of the unidirec- delivery rate. In the present study, low twisted (28 TPM) flax yarn is
tional composite samples but it is very difficult to produce a 2-dimen- used as core whereas PP is used as sheath. Initially, flax yarn having an
tional woven prepreg using the same yarn. The mechanical average Z-twist of 320 TPM has been taken for this study. It is further
performance of a wrap spun yarn mainly depends on the wrapper fed to the front delivery roller nip of a laboratory scale ring spinning
thread. During weaving, each thread is subjected to many forces in- frame and twisted in the S-direction to the pre-determined twist level.
cluding repetitive abrasive forces of the reads and heald eyes in the In this way flax yarn having Z-twist level equal to 28 TPM (as un-
loom. When a wrap spun yarn is subjected to these forces, with in few twisting below this level is not possible due to random yarn breakage) is
cycles the wrapper thread breaks. As a result, a random yarn breakage produced. The untwisted flax yarn is then fed as core in DREF 3 spin-
starts to take place during the weaving of wrap spun yarn. ning system to produce core-sheath structured flax-PP hybrid yarn. The
In our previous work, a DREF spun hybrid yarn has been developed PP slivers (sheath components) are fed from the back side of the DREF
using very low twisted flax yarn (28 twist per meter) as core and PP spinning machine. After feeding, the slivers are opened-up into in-
fibre as sheath. After analyzing different hybrid yarn properties such as dividual entity by a pinned beater and transferred to the yarn forming
tenacity, modulus, flexural rigidity and weavability, it is concluded that zone to wrap over the core flax yarn. In this way hybrid yarns of dif-
one can produce a woven prepreg in a conventional loom using these ferent core to sheath ratios are manufactured after varying the PP sliver
hybrid yarns [28]. In the present study, two different unidirectional feed rate with respect to constant core yarn feed rate of 40 m/min. A
composite structures have been developed through conventional film schematic diagram illustrating the formation of DREF spun hybrid yarn
stacking method (FSC) and through DREF yarn consolidation (DYC) is shown in Fig. 1(a). Fig. 1(b) shows a cross-sectional image of a DREF
method. In both cases, very low twisted MAgPP treated flax yarns spun hybrid yarn. Prior to DREF spinning, all flax yarns are subjected to
(28 twist per meter) are used as reinforcing component and PP, either in a MAgPP treatment. MAgPP treatment of flax yarn is performed in hank
film form or in fibre form are used as matrix forming materials. Fibre form in a boiling xylene medium at 140 °C for 5–7 min.

Fig. 1. (a) Schematic diagram of DREF spun hybrid yarn formation (b) Flax-PP (50:50) based DREF yarn cross-section.

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Fig. 2. Stacking sequences of (a) Hybrid yarn method (b) Film Stacking method.

Table 1
Particulars of the DYC and FSC composite samples.
Sample Id Variables Response

Composite Fabrication Flax: PP Void content (%)

Methodology Ratio

FSC-40 Film Stacking 40: 60 10.07

FSC-50 50: 50 11.83
FSC-60 60: 40 13.47

DYC-40 Hybrid Yarn Compression 40: 60 4.98

DYC-50 50: 50 5.69
DYC-60 60: 40 6.35
Fig. 3. Photographs of hybrid yarn based UD-Composite fabrication.

stacked yarn sample is then placed in the groove of female mold halve
2.3. Preparation of DYC and FSC unidirectional composites
as shown in Fig. 3 and subjected to consolidation after closing the mold.
During hot compression, some resin comes out from the mold through
In case of DYC unidirectional composites, DREF spun hybrid yarns
both open ends. In order to compensate the volume of matrix squeeze
are wound over a spring loaded rectangular metallic frame
out, corresponding volume of PP in film form is pre-added. In both
(25.5 cm × 19.5 cm) in a parallel configuration in layer-by-layer
cases, consolidation is carried out at 190 °C temperature, with 8 bar
manner. While in case of FSC unidirectional composites, pre-weighted
consolidation pressure and 8 bar vacuum pressure for 5 min. After
and predetermined (based on fibre to matrix ratios) number of PP strips
curing, whole set-up is cooled down to below 100 °C without releasing
having 20 mm width are placed evenly between the parallel wound flax
the consolidation pressure. The dimensions of the finally produced
yarn layers. A schematic diagram showing the stacking sequences for
composite is 20 mm (width) × 160 mm (length) × 3.5 ± 0.2 mm
both type of composites are shown in Fig. 2.
(thickness).
The stacked yarn layers are then wrapped with a thin PP film and
subsequently tied with a PP filament. The metallic frame having

Fig. 4. Tensile strength of the preliminary composite samples.

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M. Bar et al. Composite Structures 197 (2018) 63–71

Fig. 5. SEM images of (a) untreated flax fibres (b) MAgPP treated flax fibres.

Fig. 6. The cross-sectional images of hybrid yarn reinforced (DYC) composite and film stacked (FSC) composite (both composites have 50% flax content).

2.4. Experimental design speed. Specimens for flexural tests have a nominal width of 20 mm and
a span length of 56 mm. Specimens for both the tensile and flexural
In preliminary studies, it is observed that MAgPP treated flax core tests have a thickness between 3.3 and 3.7 mm and are cut in the length
based DREF yarn reinforced composites show better mechanical prop- of fibre orientation direction. The notch Izod impact behavior of the
erties than those of untreated flax yarn reinforced composites. The composite samples is tested in an impact strength tester, according to
mechanical properties of the resultant composites further improve with ASTM D256-97 test method. The specimens for notch Izod impact test
decreasing twist level of the reinforcing flax yarn. The tensile strength have a dimensions of 64 mm × 12.7 mm × 3.5 ( ± 0.2) mm. Before
of the above mentioned composite samples is reported in Fig. 4. Con- testing a V-shaped notch is engraved in all specimens using a notch
sidering the preliminary test results, very low twisted MAgPP treated cutting machine on the shoulder side of 12.7 mm dimension of the
flax yarn has been chosen as reinforcement for this study. The details of specimen or on the side parallel to the direction of the application of
all composite sample produced in this study are tabulated in Table 1. molding pressure. The notch etched on the test specimens has a notch
angle of 45 ± 1° with a radius of curvature at the apex of
0.25 ( ± 0.05) mm. The depth under the notch of the specimen is
2.5. Testing of composite samples
10.2 mm. All the tests are carried out at 27 ± 2 °C temperature and
65% RH. Each reported value represents the average of five samples.
The tensile and flexural behaviors of DYC and FSC unidirectional
composites are tested in a Zwick-Roell universal testing machine, Model
no. Z052 with 50 kN load cell attachment. The tensile properties of the 2.6. Scanning electron microscopy
composite samples are tested according to ASTM D638 test method
while the flexural behavior are tested according to ASTM D790 test Thermoplastic resin distribution in the composite structure is stu-
method. Tensile testing is carried out at 10 mm/min test speed after died using the scanning electron microscopic image of fractured com-
clamping the composite sample over an area of 40 mm × 20 mm at posite surfaces. Composite specimens are fractured cryogenically after
both ends leaving 100 mm gauge length. The strain of all composite keeping them in liquid nitrogen medium. A Small piece of cryogenically
specimens along the loading direction is measured using an ex- fractured composite surface is placed over a metallic sample holder
tensometer, model no 3560-BIA-025 M-010-ST (Epsilon Technology with the help of a double sided carbon tape and subjected to a gold
Corp, Jackson, WY, USA) of 25 mm gauze length. The reported modulus coating. After coating, the samples are examined using a scanning
is calculated at 1% strain for all composite samples. On other hand, electron microscope (SEM ZEISS EVO 50) at an accelerating 5–10 AC
flexural behavior of the composite specimens is tested at 2 mm/min test voltage.

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M. Bar et al. Composite Structures 197 (2018) 63–71

Fig. 7. SEM micrographs of the cryogenically fractured DYC (A1 and A2) and FSC (B1 and B2) composite surfaces (having 60% flax content).

Fig. 8. Tensile Stress-Strain curves of flax-PP based DYC and FSC composites. Fig. 9. Ultimate tensile strength of the flax-PP based DYC and FSC composites.

2.7. Void content dt = wf df + (1−wf ) dmat (2)

Where, wf is the fibre weight fraction and df and dmat are the fibre
The void content of the flax fibre reinforced unidirectional compo- and matrix densities respectively. The fibre weight fraction in the
site samples are determined using the following equation. composite is verified by dissolving the PP in Decalin at 160 °C.
dt −dm
V% = × 100 3. Results and discussions
dt (1)
SEM images of the MAgPP treated and untreated flax fibres, re-
Where, dt is the theoretical density of the composite samples and dm
ported in Fig. 5 state that after the treatment MAgPP forms a con-
is the measured density of the composite samples. The dm of the com-
tinuous protecting layer around the core flax. Beside this continuous
posite samples are measured using a density gradient column having a
layer, some microspheres are also observed on the MAgPP treated flax
density range 0.86 g/cc–1.30 g/cc. The density gradient column is
fibre surface. These microspheres are mainly the un-bonded MAgPP
prepared using sodium bromide with water and isopropanol [29].
particles or are bonded with the flax fibres only at their interfaces.
Whereas the theoretical density is calculated using the following
Literatures reveals that MAgPP reacts with the various functional
equation.
groups of flax fibre through ester linkage formation and enhances the

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M. Bar et al. Composite Structures 197 (2018) 63–71

of the existing literatures (on flax-PP composites) are reported within

this range. It is observed that both the DYC and FSC composites show
higher modulus than the existing reported composites which is mainly
due to better fibre orientation (because of low twisted flax yarn), better
fibre-matrix distribution (because of DREF yarn structure) and strong
fibre-matrix interphase (because of MAgPP treatment) of the present
composite structures.
At constant flax content, the DYC composites show around 10%
higher tensile strength than that of FSC composites while the FSC
composites show around 10% higher modulus than that of DYC com-
posites respectively. The void content of the FSC composites and DYC
composites are reported in Table 1. It shows that the FSC composites
have higher void content than the DYC composites. During tensile
testing void behaves as a stress concentration points which results in
low tensile strength for the composites having high void content. On the
Fig. 10. Tensile Modulus of the flax-PP based DYC and FSC composites. other hand, the higher tensile modulus (at constant flax content) of the
FSC composites than that of DYC composites is mainly attributed to
fibre-matrix bonding of the resultant composite system [30,31]. The better flax fibre orientation in FSC composites. Although, the flax yarns
preliminary study results reported in Fig. 4 also support the literatures. having same twist level are taken as initial material for both the com-
Microscopic images of both types of composite cross-sections posite structures, during DREF yarn formation the core flax fibre or-
(having 50 wt% flax) are shown in Fig. 6 where some fibre rich (yarn ientation alters due to wrapping of the sheath fibres and false twisting
bundles) zones and matrix rich (between two yarn bundles) zones are of the core [36]. This ultimately reduces the reinforcing fibre orienta-
observed in both images. However, the fibre bundles are randomly tion in the DYC composites.
distributed in DYC composite structure whereas in FSC composite, the The photographs of the tensile and compression side of the flexural
fibre bundles are arranged in a layer-by-layer manner and two parallel tested DYC and FSC composite specimens (having 50% flax) are shown
flax layers are separated by a PP layer. Hence, at constant flax content, in Fig. 11. It is observed that the damage on the compression side of the
the DYC composites have higher Fibre bundle (yarn)-Matrix interphase flexural tested composite specimen is more concentrated along the line
area than the FSC composites. of flexing in FSC while on the DYC it is more diffused. The difference in
Fig. 7 shows the SEM micrographs of the cryogenically fractured the nature of FSC and DYC composite damage is mainly due to their
DYC (A1 and A2) and FSC (B1 and B2) composite surfaces having 60% dissimilarity in fibre/matrix distribution. However, irrespective of the
flax fibre. Referring to Fig. 7, there are fibre rich regions (FRR) and composite structure a prominent line of fracture on the tensile side is
matrix rich regions (MRR) in both DYC (A1) and FSC (B1) composite observed in all composite samples.
ends. The interface of the FRR and MRR in both composite surfaces is The flexural stress-deflection curves of the DYC and FSC composites
represented by a dotted line. The enlarged view of the fibre rich region having 50% flax (same set of composites whose fracture images are
of both the DYC (A2) and FSC (B2) composite ends state that irre- displayed in Fig. 11) are shown in Fig. 12. It is observed that all flexural
spective of composite fabrication methodology the PP matrix penetrates stress-deflection curves deviate slightly from their path around 1.5 mm
in the low twisted flax yarn bundles of all composite samples. The fibres deflection level, which indicate the general specimen fracture onset (in
and the matrices in the enlarged view of the FRR of both composite general the initiation of fibre/matrix de-bonding). On further loading,
surfaces are denoted as F and M respectively. the fracture propagates and all specimens continue to take load until
The tensile stress-strain curves shown in Fig. 8 reveal that the DYC around 4 mm deflection level is reached where a sharp fall in all flex-
composites show higher breaking elongation than that of FSC compo- ural stress-deflection curves is observed which indicates the failure of
sites. This is attributed to better fibre-resin distribution in the DYC the composite specimen. The failure of FSC-composite is more or less
composites than the FSC composites leading to better load sharing be- catastrophic and goes right through the specimen while in the case of
tween the fibres in DYC composites [27]. Fig. 8 also exhibits a non- DYC-composite the matrix can still deform after the maximum and this
linearity in all tensile stress-strain curves in the form of an upturn, can be attributed to the better matrix distribution. As a result, a
which is a result of change of fibre alignment during the deformation of shoulder region is observed in the flexural stress-deflection curve of the
composites. The ultimate tensile strength and modulus of the film DYC composite while no such shoulder region is spotted in FSC com-
stacked composites and hybrid yarn compressed composites are shown posite.
in Fig. 9 and Fig. 10 respectively. In both the cases, irrespective of DYC Fig. 13 and Fig. 14 represent the flexural strength and modulus of
or FSC method of composite manufacturing, around 27% increment in the DYC and FSC composite samples respectively. Like all other fibre
composite’s tensile strength and around 36% increment in tensile reinforced composite specimen, the flexural strength of the present
modulus are observed when the flax content in the composite structures composite specimens increases with increasing fibre content. Here,
increases from 40% to 60%. The tensile modulus of different flax-PP around 30% improvement in the flexural strength is observed when the
composites reported in literatures are compared in Table 2. Comparison flax content in the respective composite specimens increases from 40%
is carried out among the composites with 40 wt% flax fibre only as most to 60%. However, at constant flax content the DYC composites display

Table 2
Comparison of tensile modulus of the flax-PP composites reported in literatures.
S. No Composite Description Flax Fibre Content (wt%) Modulus (GPa) Ref. No.

1. Flax-PP commingled yarn based Plain and twill woven fabric compressed composites 40 7.25 and 7.93 [32]
2. Ring spun yarn based unidirectional woven fabric compressed composite 40 5.8 [33]
2. Flax-PP nonwoven mat compressed composite 40 3.0 [34]
3. Flax-PP needle punched nonwoven composite made in compression molding method 40 5.3 ± 0.3 [35]
4. Film stacked composite (present study) 40 9.26.1 ± 0.4
5. DREF yarn reinforced composite (present study) 40 8.32 ± 0.2

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M. Bar et al. Composite Structures 197 (2018) 63–71

Fig. 11. Photographs of the tensile and compression sides of flexural tested DYC and FSC composites (having 50% flax content).

Fig. 12. Flexural stress-deflection curves of DYC and FSC composites (having
50% flax content).
Fig. 14. Flexural modulus of the flax-PP based DYC and FSC composites.

Fig. 15. Photographic images of the impact tested DYC and FSC composite
ends.

and DYC composites are observed at low fibre content (40%) but, the
Fig. 13. Flexural strength of the flax-PP based DYC and FSC composites.
difference becomes significant with increasing fibre content. Fibre or-
ientation plays a significant role in determining the tensile modulus of a
around 7% to 15% higher flexural strength than that of FSC composites. composite but in case of flexural modulus, the fibre-matrix distribution
It is mainly due to improved fibre- matrix distribution and low void is more important [27,39]. At lower flax content, the distance between
content of the DYC composites. As expected around 40% improvement two fibre bundles is more hence, there is no such difference in flexural
in the flexural modulus of both the types of composite specimens are modulus of the composite samples is observed. However, the distance
observed when the flax content increases from 40% to 60% respec- between two yarn bundles decreases with increasing flax content but
tively. However, no such difference in the flexural modulus of the FSC due to layer-by-layer fibre-matrix arrangement, a continuous layer of

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M. Bar et al. Composite Structures 197 (2018) 63–71

reinforcement offers better fibre orientation in composite structure. The

use of core-sheath structured yarn during composite manufacturing
reduces the effective resin flow distance which ultimately helps to re-
duce the void content and obtain better fibre-matrix distribution
leading to improved mechanical properties of the resultant composite
samples.

Appendix A. Supplementary data

Supplementary data associated with this article can be found, in the

online version, at http://dx.doi.org/10.1016/j.compstruct.2018.04.
078.

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