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DOI: 10.1016/j.jmrt.2018.12.015
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Available online 6 April 2019
Characterization of new cellulosic fiber: Dracaena reflexa as a reinforcement for polymer composite structures
P. Manimarana, S.P. Saravananb, M.R. Sanjayc,
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Corresponding authors.
, Suchart Siengchinc, Mohammad Jawaidd,
Corresponding author

Corresponding authors.
, Anish Khane
a Department of Mechanical Engineering, Karpagam Institute of Technology, Coimbatore, Tamilnadu, India
b Department of Mechanical Engineering, KIT and KIM Technical Campus, Karaikudi, Tamil Nadu, India
c Department of Mechanical and Process Engineering, The Sirindhorn International Thai - German Graduate School of Engineering (TGGS), King Mongkut’s University of Technology North Bangkok (KMUTNB), Bangsue, Bangkok, Thailand
d Department of Biocomposite Technology, Institute of Tropical Forestry and Forest Products, Universiti Putra Malaysia, UPM Serdang, Selangor, Malaysia
e Centre of Excellence for Advanced Material Research, Chemistry Department, Faculty of Science, King Abdulaziz University Jeddah, Saudi Arabia
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Received 19 October 2018, Accepted 17 December 2018
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Tables (3)
Table 1. Comparison of the physical, tensile, chemical, crystalline and thermal properties of DRFs with other natural fibers.
Table 2. FT-IR peak positions and allocations of chemical stretching in the DRF.
Table 3. Comparison of weight and atomic percentage of DRF with other natural fibers.
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The search for novel bio-fibers in the field of the green composite can rise the invention of natural fiber composite and applications. In this work, the physical, chemical, structural, thermal, tensile and surface morphology properties of Dracaena reflexa fiber (DRF) are investigated. The chemical analysis results authorized the higher cellulose (70.32%) and lesser hemicelluloses (11.02%) and lignin (11.35%) existing in DRF. XRD analysis proved that DRF has a relatively higher crystallinity index of 57.32%. The free chemical functional groups presented in DRFs were determined by FT-IR. The DRF is thermally stable up to 230°C which is greater than the processing temperature of thermoplastics resin. The C2, C3, and C5 peaks intensity of CP/MAS C13 NMR spectra once again confirmed that maximum cellulose present in DRFs. The lower density (790kg/m3) and higher tensile properties of DRF show the DRF is a suitable alternative to the synthetic fibers.

Cellulosic fiber
Dracaena reflexa
Structural properties
Thermal properties
Morphological properties
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The current interest in materials and environmental related awareness drive the researchers to use of plant fibers as substitute materials for reinforcement in polymer composites [1–3]. Plant fibers reinforced composites can be used in various fields such as automotive, packaging, marine, constructions and military because of their attractive features such as less weight, biodegradable, eco-friendly, non-toxic, less cost and better mechanical properties [4–7]. Many researchers have documented that physico-chemical properties such as density, diameter, chemical composition, thermal stability and surface roughness of the plant fibers are depending on the source of the fiber such as stem, fruit, bark, root, stalk and leaf [8,9]. The most common chemical constituents of plant fibers are cellulose, hemicelluloses, lignin, pectin and wax. The expected properties of natural fibers are lengthy, lesser diameter and low spiral angle of the cellulose arrangement. The final properties of polymer composites are depending on the type of resin, form of reinforcement (nano or micro powder, short fiber, and continuous fiber), alignment of fiber and interfacial bonding between the fiber and matrix. Different kinds of plant fibers such as Arundo Donax L., Cissus quadrangularis, banana, hemp, sisal, Grewia tilifolia and others as potential reinforcement have been examined. Some researchers recently studied suitability of natural fibers, such as Furcraea Foetida, Coccinia grandis. L and Sida cordifolia, as reinforcement for polymer composites [10–20].

In this investigation, the bio-fibers extracted from Dracaena reflexa was considered as a potential reinforcement for polymer composite. These fibers have selected for numerous reasons:

  • 1.

    It is commonly grown in all the climate conditions.

  • 2.

    Its leaves are consumed as medicine for malarial fever, poisoning, dysentery, and diarrhea and dysmenorrhea. So, it is cultivated for commercial use.

  • 3.

    Dracaena reflexa was used to clean and remove considerable amount of toxins from the air which was proved by the NASA (National Aeronautics and Space Administration).

However, there is no literature available on the fibers extracted from leafs of Dracaena reflexa. So, in this article, we analyzed physical properties, chemical composition, chemical functional groups, microstructure, thermal stability, single fiber tensile strength, crystalline properties and surface roughness of the Dracaena reflexa fiber by chemical analysis, single fiber tensile test, optical microscope, X-ray diffraction method (XRD), Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimeter (DSC), scanning electron microscopy (SEM), atomic force microscopy (AFM) and nuclear magnetic resonance spectroscopy (NMR).

2Materials and methods2.1Materials

The leafs of Dracaena reflexa plant was collected from Alanganallur town, Madurai district of Tamil Nadu, India. Dracaena reflexa is a plant native to Mozambique, Madagascar, Mauritius and other nearby islands of the Indian Ocean. It is extensively grown as an ornamental plant and houseplant which has richly colored evergreen leaves, and thick irregular stems, though it may reach a height of 4–6m.

2.2Extraction of leaf fiber from Dracaena reflexa plant

The Dracaena reflexa plants and its extracted fibers are presented in Fig. 1. The Dracaena reflexa leaves were gathered from the plant, then they were submerged into the water for retting (maximum period of two weeks). After two weeks, the fibers were mined using a comb with the metal teeth.

Fig. 1.

(a) Dracaena reflexa plant, (b) leaf, (c) water retting, (d) fibers, (e) optimal microscope image for measuring diameter.

2.3Physical analysis

It is very challenging to decide diameter of the plant fibers because the fiber is uneven in shape, so it is essential to calculate the average diameter of the fiber. With the aid of Carl Zeiss Optical microscope, the profile shapes and diameter of 25 samples of Dracaena reflexa fibers were identified. The diameter of each fiber was measured at five different places and the mean value was used for statistical analysis.

The pycnometer (toluene, ρ=866kg/m3) experimentation is an suitable technique to observe the density of the bio-fiber. First DRFs were kept in a glass container filled with silica gel for 96h to eliminate the moisture from fiber and then trim into 5mm length whiskers for put in the pycnometer. In order to remove the bubbles in the fibers, DRFs were immersed into toluene for 2h before the execution of test [21].

where, ‘ρDRF’ is the density of DRF in kg/m3, ‘ρt’ is the density of toluene in kg/m3, ‘m1’ is the mass of empty pycnometer in kg, ‘m2’ is the mass of pycnometer with fibers in kg, ‘m3’ is the mass of pycnometer with toluene in kg and ‘m4’ is the mass of pycnometer with fibers and toluene in kg.

2.4Single fiber tensile test and statistical analysis

The maximum tensile strength, Young's modulus and elongation at break of single fibers of DFFs were estimated by single fiber tensile test with aid of an Instron 5500 R UTM (Universal Testing Machine). As per the guidelines of ASTM D 3822 standard, 70mm gauge length (single fiber) and 5mm/min crosshead speed was set for experimentation. The tests were executed at a room temperature of 25°C with relative humidity of 65%. The microfibril angle (α) of DFF was determined by following the equation (2)[10].

where ‘ɛ’ represents the global deformation (or) strain, ‘α’ symbolizes the microfibril angle in degree, ‘Lo’ indicates the gauge length (mm), and ‘ΔL’ denotes the elongation at break (mm).

Commonly, tensile test results of plant fibers are scattered and depend on the age of the plant from which the fiber is extracted, extraction technique, testing environment, variation in the diameter and occurrences of defects in the surface of the fiber. It is essential to find the mean values of tensile properties through statistical analysis. Several researchers used Weibull distribution for analyzing tensile properties of cellulosic fibers. In this way, the authors performed Weibull analyzing through Minitab 17 software [17].

2.5Chemical analysis

In general, the chemical composition of the fibers was strongly affected by the region, extraction methods, soil conditions, age of the plant and approaches used, to predict the composition [15]. The aim of this examination was to quantify the amount of cellulose, hemicelluloses, lignin, wax, ash and moisture content in the DFFs. The cellulose content of DFF was assessed by using technique which explained in previous work [16]. The hemicellulose cellulose content of DFF was confirmed through neutral detergent fiber method. APPITA P11s-78 method is used to compute the lignin contents [16]. The wax percentages was proven by Conrad method [16]. For the ash content measurement the way stated by TAPPI (Technical Association of the Pulp and Paper Industry) was applied [16]. The moisture present in the DRF was assessed by electronic moisture analyzer (model MA45).

2.6Fourier transform-infrared (FT-IR) spectrum analysis

Fourier transform infrared spectroscopy (FT-IR) is the right method to detect the chemical functional group existing in the natural fiber. Particular amount of DRFs was crushed into the fine powder then blended with potassium bromide (KBr) and make pellets by applying pressure. The FT-IR spectra of DRFs obtained by a Shimadzu spectrometer (FTIR-8400S, Japan) in the wavenumber range of 4000–500cm−1.

2.7X-ray diffraction (XRD) analysis

X-ray diffraction is an excellent tool to notice the difference between amorphous and crystalline material present in the natural fiber. The examinations was done by the X’PERT-PRO diffractometer with the intensity of Cu Kα radiation wavelength of 0.154nm. The crystallinity index (CI) of the DRF was determined by using following equation suggested by Segal et al. [22].

where I002 is the intensity of crystalline peak (23°) and Iam is the intensity of amorphous peak (18°).

The crystallite size (CS) of DRF was calculate by using the following formula [23]:

where β peak's full-width at half-maximum, λ is the wavelength of the radiation (0.1541nm) and θ is Bragg angle.

2.8Thermogravimetric analysis (TGA)

It is prerequisite to verify the thermal stability of the natural fibers to confirm the fitness of fibers for high temperature composite processing and applications. Themogravimetric analysis of DRF was completed in N2 (nitrogen) environment using TGA SDT Q600 machine (TA Instruments, India) with the aid of Thermal Advantage software. The weight loss of DRF was investigated at a rate of heating 10°C/min in the temperature range of 30–1000°C. The kinetic activation energy (Ea) of the DRF is evaluated by following Broido's equation [24]:

where, R denotes the gas constant (8.32J/molK), T specify the temperature in Kelvin, y represents the normalized weight (wt/wi), wt indicates the weight of the sample at any time t, wi designate the initial weight of the sample.

2.9Differential scanning calorimeter analysis (DSC)

The differential scanning calorimetry (DSC) analysis of DRF was performed by DSC SDT Q600 (TA Instruments, India). The heating rate was retained at 10°C/min and temperature ranging from 30°C to 1000°C. ΔH is the melting peak and Tg is the glass transition temperature of DRF was finalized.

2.10Scanning electron microscopy (SEM)

TESCAN model VEGA3 scanning electron microscope with an electron beam accelerating potential of 3kV was utilized to examine surface of DRF at different amplifications. The platinum layer was formed on the surface of DRF to avoid electron beam charging influences during the examination.

2.11Energy dispersive X-ray spectroscopy analysis

Energy dispersive X-ray spectroscopy (EDX) is an excellent method to assess the quantity of elements (C, O, N, Cl, Si, etc.) distributed on the surface of DRFs in terms of weight (%) as well as atomic (%). The elements existing on the surface of the DRFs were calculated in five trials and mean value has been recorded with support of EDX (INCAPentaFETx3).

2.12Atomic force microscopy

Atomic force microscopy (AFM) can provide qualitative as well as quantities information of surface roughness parameters of natural fiber such as Ra – average surface roughness, Rq or Rrms – root mean square roughness, Rz – ten point average roughness, Rsk – skewness, Rku – Kurtosis and Rt – maximum peak-to-valley height. This analysis was executed in atmosphere environment by Park XE-100 Modal Atomic Force Microscopy. This AFM analysis has given high resolution 2D and 3D images of a surface of sample.

2.13C13 (CP-MAS) NMR spectroscopy

Solid state NMR is a helpful tool to characterize the occurrence of anisotropic (directionally dependent) interfaces in natural fiber. Solid-state NMR spectrometer (DELTA2 Modal) available at IISc, Bangalore, India was used for this investigation. This analysis was conducted in the cross-polarization mode with MAS rate of 10kHz at environmental temperature of 25°C and the operating frequency of C13 nuclei was set as 75.46MHz.

3Results and discussion3.1Physical analysis

Measurement of the bio-fiber diameter is complicated one because the fibers outer profile (diameter) is varying in nature. However, it is supposed to be circular to compute the tensile strength and Young's modulus. The diameters of the DRF is 172.5±7.897μm. Density of the natural fiber plays the virtual role in the weight of the composite . So, it is need to discover the low density novel fiber, suitably the density of DRF is 790±22.78kg/m3 which is notably lower than widely used other natural fibers such as sisal (1500kg/m3), banana (1350kg/m3), Palmyrah (1090kg/m3), Cyperus pangorei (1102kg/m3), Sansevieria ehrenbergii (887kg/m3) and Sansevieria cylindrica (915kg/m3).

3.2Single fiber tensile test and statistical analysis

The tensile properties of any natural fiber depending on chemical composition (presence of cellulose, hemicellulose and lignin), structure, growing conditions, harvesting time and extraction method. Low density fiber with improved tensile properties is preferred for lightweight composite structures. Twenty samples are tested for each gauge length ranging from 10mm to 50mm in steps of 10mm using the universal test machine (INSTRON-5500R). The tensile properties of DRF are compared with other natural fibers and are presented in Table 1. From Table 1, it can be seen that the average tensile strength, modulus and elongation at break of Dracaena reflexa fibers was higher than the some other natural fibers. It is obvious from this table that the obtained tensile strength value is about 829.6MPa. This value is higher than that found in some other natural fibers. This comparison table indicates the tensile properties of DRF are comparatively high enough for its application as reinforcement in polymer composite fabrication.

Table 1.

Comparison of the physical, tensile, chemical, crystalline and thermal properties of DRFs with other natural fibers.

Name of the natural fiber  Physical propertiesTensile propertiesChemical propertiesCrystalline propertiesThermal Properties
  Diameter (μm)  Density (kg/m3Tensile strength (MPa)  Young's modulus (GPa)  Elongation at break (%)  Microfibril angle (°)  α-Cellulose (wt%)  Hemicellulose (wt%)  Lignin (wt%)  Wax (wt%)  Moisture (wt%)  Ash (wt%)  CI (%)  CS (nm)  Thermal stability (°C)  Maximum degradation temperature (°C) 
Dracaena reflexa  176.20  790  829.6  46.37  2.95  8.5°–11.27°  70.32  11.02  11.35  0.23  5.19  6.23  57.32  19.01  232.32  348.78 
Furcraea foetida  12.8  778  623.52±45  6.52±1.9  10.32±1.6  –  68.35  11.46  12.32  0.24  5.43  6.53  52.6  28.36  320.5 
Coccinia grandis  27.33  1243  273±27.74  10.17±1.261  2.703±0.2736  13.25±0.664  62.35  13.42  15.61  0.79  5.6  4.388  52.17  13.38  213.4  351.6 
Saharan Aloevera  80.61  1325.1  805.5  42.29  2.39  11.1  60.2  14.2  13.7  1.5  7.6    56.5  5.72  225  350 
Sida Cordifolia  –  1330  703.95±23.73  42.84±2.1  2.89±0.24    69.52  17.63  18.02  0.42  8.51  2.62  56.92  18    338.2 
Acacia Arabica    1028          68.10  9.36  16.86  0.49             
Cyperus pangorei    1102  196±56  11.6±2.6  1.69    68.5    17.88  0.17  9.19  3.56  41    221  324 
Sansevieria trifasciata  80–120  1414.7  348.6  15.3  2.3                    200  315 
Mendong Grass  33.4  892  452  17.4    22.9  72.14  20.2  3.44    4.2–5.2  4.2  58.6  14.3     
Hibiscus sabdariffa.              63.5  17.5  12      51.72      275 
Borassus fruit  241.18  1256  175.52    31.34    68.94  14.03  5.37  0.64  6.83           
Agave americana    1200          68.42  15.67  4.85  0.26  7.69           
Jute  26  1300  400–773  10–30  1.5–1.8  16.9  58–63  20–24  12–15  0.5  10.99    65.8  29.25     
Rhectophyllum camerunense    947  557.1  5.8  27.5    68.2  16.0  15.6               

The Weibull distribution curves of diameter, young's modulus, tensile strength, elongation at break of DRFs were shown in Fig. 2. It can be deduced that the tensile test results of all the 20 trials were situated inside the line and fit perfectly the Weibull distribution. It can be clearly seen that the Weibull distribution with four parameters provide the mechanical properties close to the average values obtained experimentally.

Fig. 2.

Weibull distribution plot for (a) diameter, (b) tensile strength, (c) Young's modulus, (d) elongation at break of DRF.

3.3Chemical analysis

The tensile strength, thermal stability, crystallinity index (CI), non-flammability and biological decomposability of the bio-fibers are influenced by the chemical composition of that fibers. DRFs is comprised of cellulose (70.32wt.%), consisting of helically coiled cellulose microfibrils, bound together by an amorphous lignin matrix. Hemicellulose (11.02wt. %) of the DRFs was acted as a compatibilizer between cellulose and lignin. Lignin content (11.35wt. %) present in the DRFs may be act as a protection agent against the fungal attack. The Wax content of DRF is 0.23wt.% which create disturbance to interfacial bond between fibers and matrices when fabricate the composite. The moisture and ash content of DRF is 5.19wt. % and 6.23wt.% respectively. The chemical composition of DRFs was compared with that of different natural fibers and conveyed in Table 1.

3.4FT-IR spectrum analysis

The main chemical functional group presented in the DRF was detected through FT-IR spectrum is presented in Fig. 3. The peaks obtained at 3296cm−1 is corresponds to O–H stretching of α-cellulose. The peak observed at 2914cm−1 could be assigned to C–H stretching vibration of CH in cellulose component. The peak seen at 2796cm−1 shows CH stretching of hemicelluloses. The peak attained at 2357cm−1 represents C–C stretching of wax. The absorption peak at 1737cm−1 corresponds to carbonyl group (–CO) stretching vibration of the hemicellulose. The broad and strong absorption peaks noticed at 1642 and 1028cm−1 were endorsed to –CO stretching vibration of lignin. A small peak existing at 1346cm−1 represents CO stretching of hemicelluloses (Table 2).

Fig. 3.

FT-IR spectrum analysis.

Table 2.

FT-IR peak positions and allocations of chemical stretching in the DRF.

Peak positions (wave number, cm−1Functional group  Corresponding chemical constitution 
3296  OH stretching  α-Cellulose 
2914  CH stretching  α-Cellulose 
2796  CH stretching  Hemicellulose 
2357  CC stretching  Wax 
1737  CO stretching  Hemicelluloses 
1642  CO stretching  Lignin 
1346  CO stretching  Hemicelluloses 
1028  C–OH of stretching  Lignin 
3.5XRD analysis

The XRD pattern of the DRF is displayed in Fig. 4. The two enlarged diffraction peaks at 2θ=15.58° (110) and 22.41° (200), are clearly seen in most of the bio-fibers. The peak at 2θ=15.58° point out the existence of amorphous constituents in DRF. The peak at 2θ=22.31° denotes the amorphous constituents in the crystallographic plane. The crystallinity index of DRF was calculated as 57.32% which is higher than that of other bio fibers, such as C. grandis (52.17%), F. foetida (52.6%), Saharan Aloevera (56.5%), S. cordifolia (56.92%), C. pangorei (41%), Acacia leucophloea (51%), Acacia Arabica (51.72%) and lower than that of Jute (71%) and Hemp (88%). In addition, the crystallite size (CS) of the DRFs was decided as 19.01nm and higher CS minimizes the water absorption and chemical reaction ability of the fiber.

Fig. 4.

X-ray diffractogram of DRFs.

3.6Thermal analysis3.6.1Thermogravimetric analysis

Generally, bio-fiber reinforced thermoplastic composites are manufactured under the high temperature, so it is important to evaluate the thermal stability of bio-fiber at various temperatures in order to: (i) choose the exact temperature range for manufacturing of composites, and to (ii) avoid the loss of fibers properties. The thermal degradation performance of DRFs was analyzed using TG and DTA curves shown in Fig. 5(a). From TG curve it is noticed that DRF has typically four stages of degradation. The initial degradation happened from room temperature to 232.20°C with the weight loss of 11% which was associated with the elimination of moisture from the DRF. The next stage of degradation occurred from 232.20°C to 295.39 with the weight loss of 2.61% which related to the reduction of the hemicellulose of the DRF. The combined degradation of the cellulose, hemicellulose and the huge quantity of the instable materials degraded between 295.39 and 348°C with a weight loss of 51.43%. The fourth stage of degradation developed between the temperature range of 348°C and 569.96°C with a weight loss of 30.19% indicates the degradation of lignin. Comparable degradation performance was detected in the various bio-fibers such as C. grandis, F. foetida, C. pangorei and Agave Americana.

Fig. 5.

Thermal analysis: (a) TG and DTG, (b) DSC and (c) Broido's curves of DRFs.

3.7Differential scanning calorimetry

The kinetic activation energy is one of the noteworthy factor in the estimation of the thermal stability of DR fibers (Fig. 5(b) shows DSC curve). Broido's plot of DRF is shown in Fig. 5(c). From this it is clear that the kinetic activation energy (Ea) is 68.784kJ/mol. This activation energy of DRF is higher than the Coccinia grandi fiber (67.02kJ/mol), Saharan aloe vera cactus leaves fiber (60.20k J/mol) and lower than the C. quadrangularis root (74.18kJ/mol) and S. cordifolia (73.1kJ/mol).

From the above analysis it is proved that the DRFs can be potentially used as reinforcements in thermoplastic and polymers whose processing temperature is lower than 230°C.

3.8Scanning electron microscopy (SEM)

Fig. 6 shows the SEM micrographs of Dracaena reflexa fibers for morphology analysis. The figure displays a general view of cellulosic fibers with a rough surface suitable for a good bond with matrix polymer. It can be clearly seen in the figure, there is no cracks, micro voids and helical fibrils on the surface of DRFs. So it is revealed that these fibers can be used as reinforcement in polymer composite manufacturing.

Fig. 6.

SEM images of DRF.

3.9Atomic force microscopy

Fig. 7(a)–(d) shows the 3D, 2D images, line profile and parameters of atomic force microscopy analysis of DRFs. The average roughness (Ra) value of DRFs is estimated as 22.769nm which is greater than the F. foetida (18.005nm), S. cordifolia (6.712nm), Acacia planifrons (0.708nm), and lower than the C. pangorei (625nm). The higher Ra value of DRF signifies the surface of the fiber has less impurity and lignin. The roughness skewness (Rsk) value of DRF is −0875. This negative value designated that DRF surface contain lot of pores. The nature of the surface (spiky or rough) of fibers is predicted through roughness kurtosis (Rku) value. Rku value is larger than 3 indicate that is spiky surface, if it is less than 3 directs that is rough surface. The Rku value of DRF is 3.110nm which specify that surface of DRF is spiky in nature, so a slight surface modification needed to improve the surface roughness before DRF used as reinforcement in composite. Other surface parameters such as ten-point average roughness (Rz), maximum peak-to-valley height (Rt) and root mean square roughness (Rq or Rrms) of DRF were 113.013nm, 152.772nm, 28.527nm, respectively.

Fig. 7.

(a) 3-D roughness surface texture, (b) 2-D roughness surface texture, (c) 2-D line diagram for roughness measurement of DRF, (d) roughness parameters, and (e) EDX analysis of DRF.

3.10EDX analysis

Fig. 7(e) offered weight and atomic percent of elements scattered on the surface of the DRF. C (carbon), O (oxygen) and Cl (chlorine) are the existing peaks of DRF. The elements existing in of DRF and other natural fibers such as Calotropis procera, C. grandis. L, F. Foetida and sugar palm fibers were presented in Table 3. Carbon and oxygen are the major elements present in the EDX spectrum of DRF which is the usual outcome of plant fiber. DRF has 66.43% and 34.20% weight of C and O, respectively, which is more than that of C. procera, C. grandis. L and lower than F. Foetida, sugar palm fibers.

Table 3.

Comparison of weight and atomic percentage of DRF with other natural fibers.

Elements  Calotropis proceraCoccinia grandis L.Furcraea FoetidaSugar palm fibersDracaena reflexa
  Weight (%)  Atomic (%)  Weight (%)  Atomic (%)  Weight (%)  Atomic (%)  Weight (%)  Atomic (%)  Weight (%)  Atomic (%) 
61.00  67.63  44.67  51.91  66.43  72.50  87.93    65.13  71.54 
38.80  32.30  54.38  47.58  33.57  27.50  5.86    34.20  28.21 
Al  0.18  0.09   
Si  0.67  0.36  5.13   
Cl  0.2  0.06  0.38  0.06    0.67  0.25 
3.11C13 (CP-MAS) NMR spectroscopy

To verify the structural features of DRF solid state NMR (C13 NMR (CP-MAS)) experiment was conducted. Fig. 8 displays the C13 CP-MAS NMR spectrum of DRFs. Amorphous cellulose of DRF was identified at 64.074ppm (C6). The resonance peaks from 76.158 to 73.936ppm were assigned to the C2, C3, and C5 carbons ring of cellulose. Two peaks at 85.473 and 90.002ppm were endorsed to C4 carbon in the crystalline region. The peak at 22.577ppm allocated to acetyl groups of hemicelluloses. Among the peaks observed at 76.158–73.936ppm are maximum intensity which indications that higher amount of cellulose present in DRF. The comparable peaks were noticed in the several bio-fibers such as F. Foetida, Ficus religiosa, Thespesia Lampas, Napier grass and coconut fiber.

Fig. 8.

C13 (CP-MAS) NMR spectroscopy analysis.


The physico-chemical, thermal, tensile, structural and morphological properties of DRF was examined in this research work. The density of extracted DRF 790kg/m3 was vaguely increased, however, it is lower than E-glass fiber (2500kg/m3) and carbon fiber (1570kg/m3). The result of the chemical analysis and FT-IR analysis showed reduction in hemicelluloses and greater cellulose content in DRF can use as a reinforcing material in polymer matrix composite. The single fiber tensile test revealed that, the DRF also good in tensile strength and the young's modulus so it is advantageous to produce lightweight applications. From EDX analysis, it is confirmed that the carbon and oxygen were the main constituents of DRF and exposes that the fiber is organic in nature. Natural fibers with a rough surface essential feature for adhesion with polymer matrix was observed through SEM.

Conflicts of interest

The authors declare no conflicts of interest.


This research was partly supported by the King Mongkut's University of Technology North Bangkok through the PostDoc Program (Grant No.KMUTNB-61-Post-001 and KMUTNB-62-KNOW-37). The authors are also thankful to Universiti Putra Malaysia for supporting this work through HICOE Grant No; 6369108.

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Journal of Materials Research and Technology

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