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Original Article
DOI: 10.1016/j.jmrt.2018.06.013
Flexural, thermal and dynamic mechanical properties of date palm fibres reinforced epoxy composites
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Mohamed Hamdy Gheitha, Mohamed Abdel Aziza, Waheedullah Ghoria, Naheed Sabab, Mohammad Asimb, Mohammad Jawaidb,c,
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jawaid_md@yahoo.co.in

Corresponding author.
, Othman Y. Alothmanc
a College of Engineering, King Khalid University, Abha, Saudi Arabia
b Laboratory of Biocomposite Technology, Institute of Tropical Forestry and Forest Products (INTROP), Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia
c Department of Chemical Engineering, College of Engineering, King Saud University, Riyadh, Saudi Arabia
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Received 09 April 2018, Accepted 01 June 2018
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Tables (4)
Table 1. Exclusive literature reported on date palm reinforced polymer composites.
Table 2. Chemical composition of DPF.
Table 3. Formulation of DPF/epoxy composites.
Table 4. Degradation temperature and residual content of composites obtained from TGA.
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Abstract

The aim of the present study is to improve the flexural, thermal stability and dynamic mechanical properties of epoxy composites by reinforcing date palm fibres (DPF) at different loading (40%, 50% and 60% by wt.) and to evaluate the best loading through hand lay-up technique. Three point bending dynamic properties in terms of storage modulus (E′), loss modulus (E″) damping factor, Cole–Cole plot and thermal properties were analyzed by dynamic mechanical and thermogravimetric analyser, respectively. Flexural test results show that loading of 50% DPF increases both the flexural strength and modulus of pure epoxy composites from 26.15MPa to 32.64MPa and 2.26GPa to 3.28GPa, respectively. TGA results revealed that reinforcement of DPF in epoxy composites also improves the thermal stability and residual content. The residual content of epoxy (9.58%), 40% DPF/epoxy (12.51%), 50% DPF/epoxy (19.8%) and for 60% DPF/epoxy composites (15.2%) was noted, revealing that 50% DPF/epoxy composites confers the best result. Incorporation of DPF into epoxy also improves the E′ and E″ but 50% DPF show more remarkable improvement compared to 40% and 60% DPF loading. Moreover, damping factor decreases considerably by the reinforcement of DPF and are found lowest for 50% DPF/epoxy composites among all composites. Drawn Cole–Cole plot also suggests the existence of certain heterogeneity in DPF/epoxy composites compared to homogenous nature of epoxy composites. We concluded that 50% DPF loading is the ideal loading to enhanced flexural, thermal stability and dynamic properties of epoxy composites.

Keywords:
Date palm fibres
Epoxy composites
Flexural strength
Thermal stability
Dynamic mechanical properties
Damping factor
Cole–Cole plot
Full Text
1Introduction

As far as environment is concern most of the researchers are focused on the biodegradable and renewable lignocellulosic or natural fibres as the most promising material for economic growth [1,2]. Renewable resource utilizations provide the optimistic ways for sustainability of ‘green’ environment. Natural fibres such as kenaf, jute, hemp, sisal, pineapple leaf, date palm and oil palm are considered as waste material and are found abundantly throughout the world [3,4]. Although natural fibres have many advantage over synthetic fibre such as high biodegradability, non-abrasive nature, low energy consumption, low densities/cost and high specific mechanical properties [5,6]. However, many researchers reviewed that natural fibres can effectively be used as filler/reinforced material in varieties of thermoplastic and thermoset polymer composites for constructional and automotive applications [7–9].

Concerning about the date palm, the worldwide annual production of date palm tree is 42% more in comparison to coir and 20–10% more compared to hemp and sisal. Each stem of palm tree is surrounded by a mesh of single cross fibres which appears as a natural woven mat of fibres with different diameters. Most commonly, this mat is separated and cleaned to make baskets and ropes. DPF is an aggregation of 2–5μm sized multicellular fibre containing a central void and its shape and structure resembles to coir fibre [10,11]. DPF is multicellular lignocellulosic fibre containing polysaccharides cellulose (38–40%), lignin and a few minor components of fat, wax, pectin and inorganic substance [12]. Several attempts have been made to reinforce the DPF in thermoplastics and thermosets polymer to improve their physical, mechanical and thermal properties. But prior to reinforcement, usually surface modification is necessary to purify and clean the surface of the fibres from large amount of impurities and uncompleted growth, as they may result in poor adhesion between fibre and polymer. In one study, short DPF reinforced modified polyester and epoxy matrices has been reported with better morphology and enhanced mechanical properties [13]. In other study, natural weathering and thermal stability of DPF reinforced polypropylene (PP) composite materials are investigated [14]. Researchers found that the addition of DPF in the PP composites improved the interfacial adhesion and hence mechanical and thermal properties. Interestingly, these fibres are also used as effective filler in both thermosetting and thermoplastics materials [12,15,16] and their advanced industrial and engineering applications, such as automotive and airspace components were also reported in literature [12]. Some of the recently conveyed study on the date palm materials reinforced polymer composites are presented in Table 1.

Table 1.

Exclusive literature reported on date palm reinforced polymer composites.

Reinforcements  Polymer matrix  References 
Date palm fibres  Polyester  [17] 
Date palm stem fibres  Epoxy  [18] 
Date palm wood fronds  Polyester  [19] 
Date palm fibres  Polypropylene (PP)  [20] 
Date palm fibres  High density polyethylene (HDPE)  [21] 
Short date palm fibres  Poly-epoxy thermoset  [22] 
Date palm fibres  Polyester  [23] 
Date palm seed particles  Polyester  [24] 
Date seeds powder  Polyester  [25] 
Date palm fibres  PP  [26] 
Date palm leaflets  Polystyrene  [27] 
Date palm fibres and graphite filler  Epoxy  [28] 
Date palm fibres  Thermoplastic starch  [29] 
Date palm particles  Polyurethane  [30] 
Date palm fibres  Recycled PP/low density polyethylene (LDPE)/HDPE ternary blends  [31] 

From the literature survey, it is evident that no work has been reported on the incorporation of DPF in epoxy composites. The present research is aimed to explore the effect of DPF loading (40%, 50% and 60% by wt.) on flexural strength, flexural modulus, thermal and dynamic mechanical properties of epoxy composites. Besides this, it also open a platform to utilize huge deposition of DPF in the Saudi Arabian region as renewable and green reinforcing filler in polymer composite industries like other natural fibres such as kenaf, jute or hemp.

2Materials and method

Epoxy resin and hardener (Jointmine 905-3S) was supplied by Tazdiq Engineering Sdn. Bhd., Malaysia. DPF were imported from (Riyadh)-Saudi Arabia. The chemical composition of DPF shown in Table 2 was made at Malaysian Agricultural Research and Development Institute (MARDI), Selangor, Malaysia.

Table 2.

Chemical composition of DPF.

Constituents of DPF  Value (%) 
Cellulose  26.92 
Hemicellulose  43.21 
Lignin  27.42 
Extractives  1.75 
Others  0.70 
2.1Fabrication of composites

In this study DPF is used as filler for the fabrication of DPF/epoxy composites at different loading. Prior to this, DPF is ground into 0.8–1mm by using grinding machine having average 6–8% moisture content and DPF/epoxy composites were fabricated through hand lay-up technique and are tested according to ASTM standard. The ratio of DPF and epoxy in DPF/epoxy composites are listed in Table 3.

Table 3.

Formulation of DPF/epoxy composites.

Polymer composites  Epoxy resin in wt.%  DPF in wt.% 
Neat epoxy resin  100 
40% DPF  60  40 
50% DPF  50  50 
60% DPF  40  60 
3Characterizations3.1Flexural testing

Three-point bending flexural tests according to ASTM D790 standard with the crosshead speed of 2.0mm/min were applied on upper and lower surface of each six replicate specimens of pure epoxy composites and each DPF/epoxy composites and the failure was calculated when bending of specimen reach up to corresponding critical point.

3.2Thermogravimetric analysis (TGA)

Thermal stability of epoxy and DPF/epoxy composites were characterized by using a thermo-gravimetric analyzer (TGA Q500, TA Instruments, USA) at 20°C/min under a room temperature in the range of 30–700°C.

3.3Dynamic mechanical analysis (DMA)

DMA was executed according to ASTM D4065-01 to determine the viscoelastic behaviour of DPF/epoxy and pure epoxy composites as a function of temperature through TA Instruments Q800 DMA, operating at an oscillation frequency of 1Hz and temperature ranging from 30°C to 150°C with a heating rate of 5°C/min.

4Results and discussion4.1Flexural properties

Effect of loading DPF (40%, 50% and 60%) on the flexural strength and modulus on the epoxy composites are presented in Fig. 1.

Fig. 1.
(0.08MB).

Effect of DPF loading on flexural strength and modulus of epoxy composites.

From Fig. 1, the flexural strength and modulus of pure epoxy composites are 26.15MPa and 2.26GPa, respectively. However, the addition of DPF increases consecutive both flexural strength and modulus of epoxy composites up to 50% fibre loading, but beyond this loading a remarkable decrement are observed. The flexural strength and modulus at 40% DPF loading are 28.6MPa and 2.3GPa, respectively, but at 50% DPF loading both flexural strength and modulus of epoxy composites get increased up to 32.64MPa and 3.28GPa, respectively. The comparative increment in flexural strength and modulus of 50% DPF/epoxy composite with pure epoxy composites are recorded as 122.7% and 141.6%, respectively. However, at 60% DPF loading, reduction in the flexural strength (27.83MPa) and modulus (2.94GPa) of epoxy composites are noticed. Research findings reported that an increment of fibre loading in composites can increases both the flexural strength of composites up to critical loading point [8,32,33]. Decline in the value of flexural properties beyond 50% loading can be ascribed on account of insufficient quantity of available polymer matrix to wet or cover all reinforced DPF [32], resulting poor interfacial adhesion between DPF and epoxy matrix to transfer the applied stress under observation. This argument is in line with other researchers where date palm particles get agglomerates on higher loading in polyurethane matrix, due to poor wetting of the particles by the matrix besides the incompatibility due to hydrophilicity of reinforcement and hydrophobicity of polyurethane matrix [30]. Moreover, observed highest flexural strength and modulus of DPF/epoxy composites at 50% loading are also in line with other existing findings showing better flexural properties at 50% fibre loading [29,33,34].

4.2Thermal properties

Comparative TGA analysis of DPF/epoxy composites and pure epoxy composites sample was carried out in a programmed temperature range of 30–700°C are displayed in Fig. 2.

Fig. 2.
(0.09MB).

TGA plot of epoxy and DPF/epoxy composites.

Incorporation of DPF into the epoxy matrix increased the thermal stability, as evidenced by the TGA analysis in Fig. 2. In the case of DPF/epoxy composites, the first weight loss between 60 and 100°C corresponds to vaporization of water molecules or moisture content as also observed in the case of natural fibre polymer composites [35,36]. Researchers revealed that the presence of water molecule in the wall structure or void space and the water absorption at the interfacial bonding fibre–matrix [37] are ascribed for minimizing the mechanical strength of natural fibre composites [38].

From the Fig. 2 it is evident that pure epoxy composites shows relatively less weight loss at 100°C temperature, indicating the presence of less water molecules. Moreover, TGA results of pure epoxy composites and DPF/epoxy composites are summarized in Table 4. It is evidently observed that there is weight loss in all types of composites, which typically occurs in most of the lignocellulosic fibre and its composites [39–42].

Table 4.

Degradation temperature and residual content of composites obtained from TGA.

Composite samples  Degradation temperature (°C) and weight loss (%)Final residue (%) 
  (°C)  (%)   
Pure epoxy composites  305.02  65.11  9.58 
40% DPF/epoxy  299.72  70.99  12.51 
50% DPF/epoxy  316.9  75.54  19.8 
60% DPF/epoxy  281.58  74.21  15.2 

Pure epoxy composites showed 65.11% weight loss at 305.02°C and the final remaining residue was 9.58%. The degradation mechanism of an epoxy matrix can be explained on account of a two-step mechanism, starting with dehydration followed by chain scission step [43,44]. 40% DPF loading composites showed weight loss of 70.99% at the temperature of 299.72°C and final residue was 12.51%, quite more in compared to pure epoxy (9.58%), might be due to lignin content of DPF. 50% DPF/epoxy composites showed the highest thermal degradation temperature (316.9°C) and higher residual content (19.8%) or lower weight loss among all DPF loadings. But beyond 50% loading, the 60% DPF/epoxy composites also confers higher thermal degradation temperature and residual content (15.2%), but relatively less in comparison to 50% DPF/epoxy composites. Thus, it is evident that on exposure to higher temperature all DPF/epoxy composites undergoes weight loss due to the thermal decomposition of hemicellulose, lignin, pectin and the glycosidic linkages of cellulose of natural fibres [31]. However, 50% DPF/epoxy composites results better thermal stability, as the char content or the residual content at relatively higher temperature (∼700°C) is more in compared to other composites, and the higher residue content also improve the flame resistance behaviour under investigation [43].

Derivative thermogravimetric (DTG) analysis of pure epoxy and DPF/epoxy composites were also carried out to investigate derivative mass loss are shown in Fig. 3.

Fig. 3.
(0.1MB).

DTG curve of epoxy and DPF/epoxy composites.

Fig. 3 shows the decomposition temperature of each component of composites correlated with peak of DTG curves. There was only one peak located in the neat epoxy at 330°C in the DTG curve, which showed stages of degradation in the matrix with the maximum rate of degradation at 19%/min. DPF/epoxy composites exhibited two peaks; the height of the first peak was lowest, which indicates the presence of water molecules in the hemicelluloses of DPF/epoxy composites or the existence of voids that developed during the fabrication of the composites. The heights of the second peak of the DPF/epoxy are higher indicating that all DPF/epoxy composites decomposed at a relatively higher temperature compared to pure epoxy, however, 50% DPF/epoxy decomposed at relatively higher temperature among all. Moreover, Fig. 3 also revealed that derivative weight loss of epoxy composites was relatively higher with respect to all DPF/epoxy composites, while 50% DPF/epoxy displayed the minimal derivative weight loss. The observed result are also in agreement with other researches, where DPF and flax fibres are reinforced at total 50% loading in biodegradable starch-based composites [45].

4.3Dynamic mechanical properties4.3.1Storage modulus (E′)

The E′ vs. temperature were plotted to extract important information about stiffness, fibre/matrix interfacial bonding and degree of cross linking of materials [46]. E′ contributes to elaborate elasticity of composite components and has three region namely glassy region, transition region and rubbery region [47]. Fig. 4 display the effect of different DPF loading (40%, 50% and 60% by wt.) on E′ of epoxy composites.

Fig. 4.
(0.09MB).

Storage modulus of epoxy and DPF/epoxy composites.

Research study declares that in the glassy region, composite components are in highly compact and frozen stage resulting high E′ value [48]. Beyond glass transition region, E′ of all composites decreases considerably due to increase in mobility of polymer chain above Tg temperature [49] and defined the rubbery region. From the Fig. 4, it is also evident that incorporation of DPF in epoxy composites improves the E′ of pure epoxy composites, however, it marginal increment in 40% DPF loading in the glassy region indicating that fibre loading did not confers much effect in the molecular mobility of the polymer chains above Tg [50]. Furthermore, E′ of epoxy composites get improved after the addition of fibres up to 50% representing the higher stiffness and perfect distribution of DPF within epoxy matrix of developed composites. But further increment of DPF content beyond 50% showed noticeable reduction in modulus chiefly ascribed due to weak fibre/matrix adhesion, unevenly dispersion and agglomeration of DPF within epoxy matrix which might reduce the reinforcing effect of fibre as filler in composites [51]. Recently research study reported that the thermal properties of pineapple leaf fibre and kenaf fibre of total 50% fibres loading in phenolic composites also exhibits highest E[52].

4.3.2Loss modulus (E″)

The loss modulus curve is the measure of energy dissipated as heat per cycle under deformation experienced in a viscoelastic material [47]. Fig. 5 presents the effect of different DPF fibre (40%, 50% and 60% by wt.) loading on loss modulus of epoxy composites.

Fig. 5.
(0.1MB).

Loss modulus of epoxy and DPF/epoxy composites.

Fig. 5 clearly shows that E″ plot follows somehow the same trend as E′ verses temperature, showing improvements by the incorporation of DPF. Furthermore, all E″ curves reach a maximum values for maximum dissipation of mechanical energy and decreases for higher temperatures, as a result of the free movement of the polymer chains. From Fig. 5, it is clearly evident that the pure epoxy display narrow peak in the range of temperature 70–80°C. However, the addition of DPF in the epoxy matrix improved the loss modulus peak height of epoxy composites, since the ranges of peak express the diversity of chain segment of polymer three-dimensionally [53]. Broadening the curve of the polymer matrix after the addition of DPF indicated that fibre played an important role above Tg. The broadening in E″ is due to enhancement in chain segment as well as more free volume with the addition of natural fibres [54]. Interestingly, the difference in E″ of 40% and 60% DPF/epoxy composites are marginal, however, 50% DPF loading shows improved E″ may be due to better adhesion of matrix with fibres. The highest E″ peak height of 50% DPF/epoxy also indicates the possibilities of its higher mechanical properties compared to epoxy composites and among all DPF/epoxy composites. Similar arguments and observations are observed in the case of kenaf hybrid composites [55].

4.3.3Damping factor

Fig. 6 illustrates the damping factor of the pure epoxy and different loading (40%, 50% and 60% by wt.) of DPF/epoxy composites plotted vs. temperature. It is evidently clear that the incorporation of DPF at all loadings influenced the damping factor of epoxy composites.

Fig. 6.
(0.09MB).

Damping factor of epoxy and DPF/epoxy composites.

It was also observed that, damping factor reaches maximum in a transition region and then reduced dramatically in a rubbery region. This phenomenon represent the initial frozen stage before Tg and then mobility of small groups of materials/or molecules within polymer structure after glass transition region [46]. Moreover, epoxy composites showed higher peak value of damping factor indicating higher degree of molecular mobility [56] compared to the rest DPF/epoxy composites. But the addition of DPF in epoxy substantially decreases the viscoelastic damping factor as because epoxy resin is known as bad thermal resistance and higher thermal resistant polymers used to have minimum degree of molecular mobility [57,58]. Remarkably 50% DPF reinforced epoxy composites shows lower damping factor while 40% DPF/epoxy composites convey highest among the rest DPF reinforced epoxy composites. Moreover, peak of dynamic damping of epoxy composites also get broader due to incorporation of DPF indicating the higher crosslinking density in all DPF/epoxy composites [55]. A wider peak of dynamic damping are observed for 50% DPF/epoxy, revealing the existence of more time for relaxation of molecules due to lower polymeric chains movement due to better interfacial interaction. Researcher reported in the literature that in case of fibres reinforced polymer composites, the damping peak height appear due to fibre's internal energy dissipation between fibre/matrix inter-phase [59].

4.4Cole–Cole plot

Cole–Cole also referred as Wicket plot is the highly valuable method to interpret the relationship between E′ and E[47]. Homogenous curves indicated by smooth, semicircular arc, while imperfect or irregular shape signifies the heterogeneity in the polymeric system [41]. Fig. 7 displayed the Cole–Cole plot where the E″ data are plotted as a function of E′ for all epoxy composites. It is evident from Cole–Cole curve that epoxy composites have relatively lowest heterogeneity revealing its brittle nature.

Fig. 7.
(0.11MB).

Cole–Cole plot of epoxy and DPF/epoxy composites.

While the addition of DPF in epoxy reduces its homogeneity and increases heterogeneity, associated with greater differences in the relaxation process of incorporated DPF. Interestingly, 40% DPF loading shows almost similar semi-circular and smooth arc, indicating perfect distribution in the epoxy matrix. However, in the case of 50% DPF loading the graph shows great deviation from semi-circular, but still delivers a very smooth semi arc plot without any upward inflection. But at 60% loading, there is a clear deviation from semi-circular shape showing irregular arc which indicates immiscibility or aggregation of DPF resulting poor interfacial interaction. All this contributes to irregular and modified semi-circular arc in Cole–Cole plots. Overall, 50% DPF loading found optimal with perfect interfacial bonding between epoxy and reinforcement providing high E′ and thermal stability.

5Conclusion

This study deals the successful incorporation of DPF at different fibres loading to enhance the flexural, thermal and dynamic properties of epoxy composites. Both flexural strength and modulus of epoxy composites get enhanced by the addition of DPF, however 50% DPF loading shows better improvement compared to the rest of composites, ascribed on the basis of better dispersion, wetting of fibres and interfacial bonding between DPF and epoxy matrix. TGA and DTG analysis also exposed that 50% DPF loading improved the thermal stability and residual content, explained on account of better compatibility and adhesion in which polymer acts as a barrier to prevent the degradation of fibres. Furthermore, remarkable improvement in E′ and E″ for 50% DPF loading, whereas noticeable reductions beyond 50% in these dynamic properties are observed. Besides this incorporation of DPF also results considerable reduction in mobility hence reduces the damping factor of all DPF/epoxy composites relative to pure epoxy composites.

The success of this work probably minimize huge date palm wastes deposition and could provide an attempt to lower the existing use of synthetic fibres in polymer composite industries for advanced engineering applications such as in automotive, paper making and outdoor applications.

Conflicts of interest

The authors declare no conflicts of interest.

Acknowledgments

This work is funded by Deanship of Scientific Research, King Khalid University, Abha, The Kingdom of Saudi Arabia, Project No. (499) and the authors express their gratitude to King Khalid University for supporting this research work.

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Journal of Materials Research and Technology

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