Thermal and mechanical characterisation of Phormium tenax-reinforced polypropylene composites
Transcript of Thermal and mechanical characterisation of Phormium tenax-reinforced polypropylene composites
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DOI: 10.1177/0892705712473629
published online 20 February 2013Journal of Thermoplastic Composite MaterialsD. Puglia, C. Santulli, F. Sarasini, J.M. Kenny and T. Valente
polypropylene compositesThermal and mechanical characterisation of Phormium tenax-reinforced
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Article
Thermal and mechanicalcharacterisation ofPhormium tenax-reinforcedpolypropylene composites
D. Puglia1, C. Santulli2, F. Sarasini2,J.M. Kenny1 and T. Valente2
AbstractComposites including short and randomly arranged Phormium tenax fibres in a poly-propylene (PP) matrix (fibre content of 20, 30 and 40 wt%) were produced by twin-screwcompounding and injection moulding. They have been characterised by tensile testing,scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and differentialscanning calorimetry (DSC). The results indicated that tensile modulus has been increasedby reinforcing the matrix with growing amounts of fibres, whilst the effect on tensilestrength had lower evidence. Fracture surface characterisation by SEM indicated thatdebonding and pull-out are prevalent, which suggests the need to optimise the interfacialbonding. Thermal characterisation results have shown that the main degradation peak forPP was slightly shifted to higher temperatures with the increasing fibre contents, thusimproving the thermal stability of the composites. The introduction of fibres did not resultin a significant variation in the position of the peaks for calorimetric analysis, except for themelting peak, which appeared lower for the composites with respect to the neat matrix.A slight increase in crystallinity was also measured.
KeywordsThermoplastic composite materials, mechanical properties, thermal characterisation,natural fibres, Phormium tenax
1 Materials Science and Technology, Civil and Environmental Engineering Department, Universita di Perugia,
Terni, Italy2 Department of Chemical Engineering Materials Environment, Sapienza – Universita di Roma, Roma, Italy
Corresponding author:
C. Santulli, Department of Chemical Engineering Materials Environment, Sapienza – Universita di Roma, Via
Eudossiana 18, Roma 00184, Italy.
Email: [email protected]
Journal of Thermoplastic Composite
Materials
1–11
ª The Author(s) 2013
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DOI: 10.1177/0892705712473629
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Introduction
The depletion of petroleum resources coupled with the adoption of stricter environ-
mental regulations is stimulating the search for materials and products with the lowest
possible environmental ‘footprint’. In this regard, biocomposites made from natural
fibres and oil-derived thermoplastic polymers, for example, polypropylene (PP) and
polyethylene (PE), can represent a suitable alternative to glass fibre-reinforced compo-
sites, providing potential value-added source of income to the agricultural community,
without extensively modifying the fabrication processes for the composites.1,2 In this
field, the use of thermoplastic composites offers several advantages compared with
that of thermosetting ones, normally including high impact resistance, damage toler-
ance, low price and easier recyclability of the polymer matrix. Currently, the main
areas of application of thermoplastic natural fibre composites are packaging, transpor-
tation and building industries. The use of non-biodegradable thermoplastic polymers as
matrix for natural fibre composites can also be intended as a step towards the applica-
tion of natural and biodegradable polymers, such as poly(lactic acid),3 polycaprolac-
tone4,5 and poly(b-hydroxybutyrate-co-valerate),6 which are being considered as
matrices for the next generation of ‘green’ composites.
PP is perhaps the most commonly used polymer to produce thermoplastic natural
fibre composites, even though other synthetic polymers, such as PE, polystyrene and
polyamides, are also common in natural fibre composites. Of all thermoplastics, PP
shows the highest potential benefits when combined with natural fibres for making
composites of industrial value.7 Several types of natural fibres have been investigated in
PP, including bast fibres such as flax,8 hemp,9 kenaf,10 jute,11 ramie,12 abaca,13 vetiver,14
leaf fibres (sisal,15 date palm16 and pineapple17) and coconut fruit skin fibres (coir18).
The resulting composites and properties have also been recently reviewed.19 Amongst
natural fibres, leaf fibres appear promising for obtaining long stretches of aligned fibres.
In case of the most used leaf-extracted fibres, that is sisal, PP matrix resulted particularly
suitable to the fabrication of composites: a number of aspects were investigated in the
literature, which included mechanical properties and effects of fire retardants20 and rheo-
logical behaviour.21
In recent years, a renewed interest has been shown for fibres extracted from the leaves
of the Phormium tenax,22,23 commonly known as harakeke or New Zealand flax, a
monocotyledonous plant which is endemic to New Zealand. Harakeke is a significant
source of fibre that has a traditional use by the Maori people as a fibre for weaving mats
and ropes.24 The use of Phormium fibres as reinforcing system in plastics has often been
proposed, in thermosets,25–28 thermoplastics29 and biodegradable thermoplastics.30–32
Thermoset-based composites are well characterised; however, limited data are still avail-
able on non-biodegradable thermoplastic-reinforced composites. In order to extend the
potential applications of P. tenax fibres, a detailed mechanical and thermal characterisa-
tion of these composites is needed.
To this purpose, this experimental work is aimed at investigating the use of untreated P.
tenax fibres as reinforcement in PP matrix. This is considered preliminary to the appli-
cation of possible compatibilisation treatments, such as maleic anhydride, to the matrix
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and is aimed in particular at the comparison of the composite properties with what has been
obtained using untreated P. tenax fibres in thermosetting matrices.28 Several properties
including mechanical and thermal properties were studied. The morphologies of the
fractured specimens were also investigated using a scanning electron microscope (SEM).
Materials and testing methods
Materials
PP homopolymer (Moplen HP 501-L) was supplied by Lyondell Basell (Ferrara, Italy).
As per supplier’s data, HP 501-L has the following properties: melt flow rate is 6 g/
10 min (230�C/2.16 kg), density is 0.9 g/cm3, tensile stress at yield is 34.0 MPa, tensile
modulus is 1500 MPa and tensile strain at break exceeds 50%. P. tenax fibres were col-
lected from New Zealand. Leaves were stripped and the hanks of fibres were washed and
then paddocked and scutched, according to the typical procedure followed for these
fibres.23 The fibres were cut to a length of 2–3 mm.
Composites manufacturing
PP composites were manufactured using a twin-screw microextruder (DSM Explore
5&15 CC Micro Compounder), and the mixing process parameters (100 r/min screw
speed, 1 min mixing time and the temperature profile would be: 170–180–190�C) were
modulated in order to optimise the final properties of material. To obtain the desired spe-
cimens for the characterisation, the molten composite samples were transferred after
extrusion through a preheated cylinder to a mini injection mould (Tmould ¼ 25�C,
Pinjection ¼ 8 bar). Composites were prepared with different amount of Phormium fibres:
specifically, a masterbatch containing 40 wt% of Phormium fibres was prepared
(PP40PH), whilst the other compositions (20 and 30 wt%, designed as PP20PH and
PP30PH, respectively) were obtained diluting the master with neat PP.
Tensile tests
Tensile tests were performed in accordance with the UNI EN ISO standard 527/2: the
type IBA (ISO 527-2 type 1BA tensile test specimens) sample was used for tensile
testing with an initial grip length of 5 mm. Loading was applied in displacement control,
using a load cell of 30 kN by means of a digital Lloyd Instrument LR 30K (Segensworth
West, Foreham, UK) with a crosshead speed of 5 mm/min. Average tensile strength,
percentage deformation at break and elastic modulus were calculated from the resulting
stress–strain curves. The measurements were performed at room temperature and at least
five samples were tested, expressing the results as mean value and SD.
Thermal and morphological characterisation
Thermogravimetric analysis (TGA) was performed on a 10-mg sample on a Seiko Exstar
6000 TGA quartz rod microbalance (Seiko Instruments, Inc., Chiba, Japan). The tests
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were carried out in nitrogen flow (250 ml/min) from 30 to 900�C with a 10�C/min heat-
ing ramp.
Differential scanning calorimetric (DSC TA Q200,TA Instruments, Vimodrone,
Italy) measurements were performed in the temperature range from �25 to 250�C, at
10�C/min, performing two heating and one cooling scans. The peak temperatures for
melting and crystallisation were evaluated and the degree of crystallinity of the sample
was calculated taking as reference 191.3 J/g as heat of melting of the fully crystalline
sample according to the following equation33
Xc ¼�Hm
�H0mð1� wfibreÞ ð1Þ
where �Hm is the enthalpy of melting (Joules per grams (J/g)), �H0m is the enthalpy of
melting for 100% crystalline PP (J/g) and wfibre is the weight fraction of Phormium
fibres.
A Philips XL40 SEM (Eindhoven, The Netherlands) was used to investigate the
fracture surfaces of the composites. Prior to observation, the specimens were gold coated.
Results and discussion
To allow a sound comparison with strength and stiffness of the composites, it is note-
worthy recalling the values obtained elsewhere in a study on the tensile properties of
Phormium fibres.22 To summarise the results obtained in De Rosa et al.’s study,22 average
strength was progressively reduced, passing from 20 to 40 mm grip length, from a value of
770.68 to 465.96 MPa, whilst average Young’s modulus increased from 23.89 to
27.59 GPa, in both the cases with substantial coefficients of variation, in the region of 40%.
Figure 1 and Table 1 show typical tensile curves and properties for neat PP and PP/
Phormium composites, respectively. The results indicate that Young’s modulus
increases with increasing Phormium content. Tensile modulus has been consistently
increased by reinforcing the composite with growing amounts of fibres, whilst the effect
on tensile strength is less evident, as is the case in a large number of lignocellulosic fibre
composites. This increment in the modulus is in agreement with the findings from the
literature,26,27 where adding fibres to a thermoplastic polymer restrains the movement of
its chains, thereby increasing the stiffness. The addition of Phormium fibres did not
largely improve the tensile strength: this is also a common trend for natural fibre-
reinforced composites. It needs to be noted, however, that the addition of a 20% of short
untreated Phormium fibres to a thermosetting matrix resulted elsewhere in a consider-
able reduction in tensile strength.28
This behaviour is usually an indication of poor adhesion between natural fibres and
polymers and, as a consequence, of not very effective stress transfer across the interface.
Generally, tensile strength is much more dependent on the interfacial adhesion than the
Young’s modulus is.27
The morphology of the fracture surface of the injection-moulded specimens resulting
from the tensile tests was investigated using SEM to characterise the fracture behaviour
of PP/Phormium composites (Figure 2(a) to (f)).
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From micrographs, it is evident that debonding and pull-out (Figure 2(a), (b), (e) and
(f)) dominate the fracture surface, thus confirming the poor interfacial bonding as pro-
posed in the discussion. Phormium fibres show a surface with no clear signs of resin
or resin particles adhering to it (Figure 2(a)) and finite gaps near the interfacial region
are present (Figure 2(b), (e) and (f)): both these evidences indicate a poor adhesion
between filler and matrix. It is also to be noted that a number of lumens appear to be
completely filled (Figure 2(d)) and the occurrence of some fibre breakage in the plane
of fracture (Figure 2(c) and (d)) suggest that some degree of adhesion has been achieved.
Despite this, as a general comment, the interface would need to be optimised for a more
effective use of the composite.
Table 1. Summary of mechanical properties of neat PP and PP/Phormium composites.
Materials Tensile strength (MPa) Young’s modulus (GPa)
PP 35.24 + 0.26 1.94 + 0.17PP20PH 36.13 + 0.50 2.94 + 0.25PP30PH 35.80 + 0.48 3.22 + 0.38PP40PH 36.45 + 0.54 4.19 + 0.36
PP: polypropylene.
Figure 1. Typical tensile curves for neat PP and PP/Phormium composites. PP: polypropylene.
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This is also a common trend of PP composites including lignocellulosic fibres, which
was also revealed using aspen fibres,34 using jute fibres35 and using coir fibres36; the
effect of poor wettability of the fibres36 becomes more severe for higher fibre contents.
In this respect, the results obtained with untreated Phormium fibres in PP do appear quite
promising for the further application of a limited amount of chemical treatments.
The thermal stability of neat PP- and PP-based composites was investigated in terms
of weight loss as a function of temperature by TGA. In Figure 3(a), TGA thermograms
and in Figure 3(b) DTG curves are reported for PP and PP/Phormium composites. An
enlarged view of TGA of the Phormium fibres is also provided between 150 and
Figure 2. Scanning electron micrographs of (a–d) PP 40 wt% Phormium composites; (e and f) PP30 wt% Phormium composites. PP: polypropylene.
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200�C (Figure 3(c)), which indicates that the mass decrease is very limited, so as to show
that the fabrication of the composite, involving the application of a 190�C heating pro-
cess for 1 min, does not lead to a substantial degradation of the Phormium fibres.
In P. tenax fibres, the decomposition occurs in two main stage processes as shown in
Figure 3(b).11 The first stage process (200–305�C) is the thermal depolymerisation of
hemicellulose, pectin and the cleavage of glycosidic linkages of cellulose;11 the second
stage process (305–370�C) is attributed to the decomposition of the a-cellulose,11 whilst
the decomposition of lignin occurred slowly within the whole temperature range. This
(a) (b)
0
20
40
60
80
100
0
0.01
0.02
0.03
0.04
0.05
0.06
0.07
0.08
100 200
150 160 170 180 190 200
300 400 500 600 700 800 900
TG
DTG
Res
idua
l mas
s (%
) DT
G (µ
g/µgi m
in)
Temperature (°C)
85
85,2
85,4
85,6
85,8
86
Untreated phormium
Res
idua
l m
ass
(%)
Temperature (°C)
(c)
Figure 3. Residual mass (a) and differential residual mass (b) obtained from the TGA analysis forneat PP and PP–Phormium composites and (c) Phormium fibres. TGA: thermogravimetric analysis;PP: polypropylene.
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was attributed to the complex structure of lignin. According to the TGA curve of the
fibre and not considering the moisture loss at the beginning of the test, the char residue at
600�C of the fibre is approximately 33 wt%. Neat PP has the degradation peak at 460�C:
this was shifted to higher temperatures for the 20, 30 and 40 wt% PP/Phormium com-
posites (Figure 3(c)). Therefore, the system fibre–matrix degrades later than the neat
resin. As a consequence, the thermal stability of the composite is slightly higher than that
of fibre and matrix. It is also evident from Figure 3(a) that residual mass at the end of the
test increases with the fibre content, since the char residue of the Phormium-based
composites at 600�C is higher for the PP40PH system with higher fibre content. The char
value at this temperature for the composites is comparable with the theoretical char
residue obtained from the combustion of the fibre at different weight contents in the
same test condition.
From the point of view of DSC characterisation, the introduction of fibres did not
result in a significant variation in the position of the peaks, except for the melting peak,
which appears lower for the composites with respect to the pure matrix. A slight
increase in crystallinity was also measured, as detected from the measurements of
crystallinity in the second heating scan (Xc ranged from 47.3% to 58.4% for the neat
resin and PP 40 wt% Phormium composites, respectively). In Figure 4, which shows
DSC thermograms obtained from the cooling scan, the nucleating effect of fibres is
evident.
In general, the introduction of short-untreated P. tenax fibres in PP composites does
compare well with that of other lignocellulosic fibres in non-biodegradable thermoplas-
tic matrices, which indicates some potential for their use in semi-structural large volume
Figure 4. Heat flow for the second heating (a) and the cooling cycle (b) obtained from the DSC forneat PP- and PP-based composites. DSC: differential scanning calorimetry. PP: polypropylene.
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applications. This is suggested by the fact that the mechanical properties of the compo-
site do not decrease with respect to the neat polymer, despite the fibres are not compa-
tibilised to provide a sound interface with PP.
Conclusions
This work on composites obtained introducing P. tenax fibres in a PP matrix gives
promising results for the applicability of these composites, where a larger stiffness and
increased thermal stability are required. In general, using short Phormium fibres in a
randomly oriented arrangement did result in a highly positive effect on composite tensile
modulus and thermal stability and in a limited modification of tensile strength and of the
thermal profile of PP. The main area of concern for these composites appears to be
represented by the need to improve the interface strength, since at higher fibre content, a
weak fibre–matrix link leads to diffuse fibre pull-out and debonding. Future studies will
involve a comparison of these results with those obtained by compatibilising the matrix
with the fibre, for example, by maleic anhydride grafting.
Funding
This research received no specific grant from any funding agency in the public, com-
mercial, or not-for-profit sectors.
Acknowledgement
The authors acknowledge the contribution of Dr Antonio Iannoni to the manufacturing of
the composites tested in this work.
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