International Journal of Biological Macromolecules 142 (2020) 212–221

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International Journal of Biological Macromolecules

journal homepage: www.elsevier.com/locate/ijbiomac

Characterization of a new cellulosic natural fiber extracted from the root

of Ficus religiosa tree
A. Arul Marcel Moshi a,⇑, D. Ravindran a, S.R. Sundara Bharathi a, S. Indran b, S.S. Saravanakumar c,
Yucheng Liu d,e
a
Department of Mechanical Engineering, National Engineering College, Kovilpatti 628 503, Tuticorin District, Tamil Nadu, India
b
Department of Mechanical Engineering, Rohini College of Engineering & Technology, Palkulam, Kanyakumari District, Tamil Nadu 629 401, India
c
Department of Mechanical Engineering, Kamaraj College of Engineering and Technology, Virudhunagar, Tamilnadu, India
d
Key Laboratory of Bionic Engineering (Ministry of Education, PR China), Jilin University (Nanling Campus), Changchun 130022, PR China
e
Editorial Department of Journal of Bionic Engineering, Jilin University (Nanling Campus), Changchun 130022, PR China

a r t i c l e i n f o a b s t r a c t

Article history: Physical, chemical, thermal and crystalline properties of new natural fiber extracted from the root of Ficus
Received 20 May 2019 Religiosa tree(FRRF) are reported in this study. The chemical analysis and X-ray diffraction (XRD) analysis
Received in revised form 4 September 2019 results ensured the presence of higher quantity of cellulose content (55.58 wt%) in the FRRF. Nuclear
Accepted 12 September 2019
Magnetic Resonance (NMR) spectroscopy analysis is transported away to support the chemical groups
Available online 13 September 2019
present in the considered fibre. Thermal stability (325 °C), maximum degradation temperature (400 °C)
and kinetic activation energy (68.02 kJ/mol.) of the FRRF areestablished by the thermo gravimetric anal-
Keywords:
ysis. The diameter (25.62 lm) and density (1246 kg/m3) of the FRRF have been found by the physical
Ficus Religiosa root fiber (FRRF)
Atomic force microscope analysis (AFM)
analysis. Scanning electron microscope analysis (SEM) and Atomic force microscope analysis (AFM) out-
NMR Spectroscopy comes revealed that FRRF has the relatively smoothest surface. Altogether the above outcomes proved
that novel FRRF is the desirable reinforcement to fabricate the fiber reinforced composite materials.
Ó 2019 Elsevier B.V. All rights reserved.

1. Introduction the stem of Cissus Quadranglaris plant (CQF); and detailed that
the fiber has lower density (1.22 g/cm3) in comparison with that
Baskaran et al. Characterized a new natural fibre extracted from of synthetic fibers such as glass and carbon fibers. CQF has the bet-
the bark of Dichrostachys Cinerea(DCF). They reported that the pro- ter tensile strength and thermal stability (270 °C) [5]. Jayaramudu
posed DCF has significant thermal stability up to 226 °C tempera- et al. investigated the fibers obtained from the bark of Grewia
ture; in turn DCF can be used as a better reinforcement for high Tilifolia tree (GTF). The morphological study showed that the GTF
temperature polymer matrix applications [1]. Belouadah et al. has uni-axially aligned constituents with rough surface. After
studied thefibre extracted from the stemof the Lygeum Spartum carrying out the entire characterization process, the authors said
plant (LSF). The results disclosed that the LSF had significant rough that the GTF could be proposed for producing the high strength
surface which is the desirable property to achieve good interfacial composite structures [6].
bonding between the fiber and matrix [2]. Gopinath et al. charac- Mabrouk Maache et al. worked with the Juncus Effusus fiber (JEF)
terized the fiber extracted from the stem of the Sida Rhombifolia obtained from the stem of the plant. It was noted from the thermo-
plant (SRF). SRF had higher value of crystallinity index as 56.6%, gravimetric analysis results that the JEF has the thermal stability
which indicated the fiber had rich cellulose contents, in turn high upto 220 °C, in turn the fiber is preferable for high temperature
crystalline nature [3]. Rajesh Jesudoss Hyness et al. verified the applications [7]. Maepa et al. reported from the characterization
fundamental properties of the plant fiber obtained from the tip resultsof fiber obtained from the top stem of raped Maize Tassel plant
of the Heteropogon Contortus plant (HCF). The HCF would have a (MTF) that the MTF yield great mechanical properties since they are
lesser density (602 kg/m3) and greater tensile strength composed of the highest percentage of cellulose contents (41%) and
(476 ± 11.6 MPa) [4]. Indran et al. extracted the bio- fiber from comparable lower amount of hemicelluloses (29%) and lignin (18%)
constituents [8]. Maheshwaran et al. analyzed the Epipremnum Aur-
eum fibers (EAF) for checking out the possibility of using them for
⇑ Corresponding author. reinforcement material for composite materials. From the thermal
E-mail address: moshibeo2010@gmail.com (A. Arul Marcel Moshi).

https://doi.org/10.1016/j.ijbiomac.2019.09.094
0141-8130/Ó 2019 Elsevier B.V. All rights reserved.
 A. Arul Marcel Moshi et al. / International Journal of Biological Macromolecules 142 (2020) 212–221 213

stability analysis and SEM analysis, it was understood that the fibers From the literature study, it was understood that the characteri-
have ahigh range of thermal stability upto 328.9 °C, and the fiber zation of new natural fiber holds more importance in the field of
surface is significantly rough for better bonding with the polymer composites since that helps to identify the suitability of using them
matrix [9]. Prithivraj et al., analysed the fibers of Perotis Indica plant in preparing composite structures for different critical applications.
(PIF). The density of the PIF was determined with the help of pyc- By getting motivated from the literatures on the characterization
nometer set up, and the value was obtained as 785 kg/m3, which is works, a new cellulosic natural fiber has been identified from the
lower than that of other natural fibers [10]. Manimaran et al. ana- root of Ficus Religiosa tree and the characterization work was carried
lyzed the properties of Red Banana Penduncle (RBPF) to be used as out.
a better reinforcement with high strength composite materials.
The higher value of cellulose content (72.9%) and high crystallinity
index (72.3%) value justified that the (RBPF) is best fitted for creating 2. Materials and methods
composite structures with high specific strength [14]. Vijay et al.
characterized the Tridax Procmbens fibers (TPF). The X-Ray diffrac- 2.1. Materials
tion analysis showed that the crystalline size of the TPF is
25.04 nm. The authors stated that the strength of the fiber material The Ficus Religiosa tree also known as Peepal tree normally grows
can be improved by increasing the cellulose contents and also up to 30 m height, which has the lifespan of 900–1500 age. This tree
decreasing the hemicellulose, wax and lignin contents with the aid is native to India. However, it is distributed in the various regions of
of chemical treatments [16]. Shanmugasundaram et al. had a work the world such as China, Nepal, Pakistan, Thailand, Bangladesh,
on characterizing the Areca Palm Leaf Stalk fiber (APLSF). The Bhutan, Egypt, Madagascar, America and Australia.
researchers analysed the surface roughness value of the APLSF sur-
face by means of Atomic Force Microscope (AFM). The results 2.2. Extraction of fiber from the tree
revealed that the surface of the fiber had a smooth surface[22]. M.
Kathirselvam et al. extracted and characterized the fibers from the The roots of Ficus Religiosa tree were collected from M.Kallupatti
bark of Thespesia Populnea plant (TPF). The AFM micrograph results village, Madurai District of Tamilnadu, South India; and the fiber
indicated that the APLSF surfaces have porous sections, which were was extracted by microbial degradation for the 15 days. After that,
confirmed with the help of SEM images [23]. the immersed roots were taken out of the water and thoroughly

Fig. 1. (a) Ficus Religiosa tree (b) Extracted FRRF (c) Optical microscopic image of FRRF.
214 A. Arul Marcel Moshi et al. / International Journal of Biological Macromolecules 142 (2020) 212–221

13
cleaned with the help of fresh water. Followed by, the roots were 2.5. C (CP-MAS) NMR spectroscopy
dried in direct sunlight about a week of time in the position of pro-
gressing to the fibre with free of moisture capacity. The tree from Solid state Carbon 13 Nuclear Magnetic Resonance 13C (CP-
which the fibers got collected, the extracted fibers and the micro- MAS) NMR spectroscopy has been used to confirm the chemical
scopic image of a fiber are shown in the Fig. 1(a)–(c) respectively. structure of the proposed natural fiber [24]. The test has been per-
formed at the room temperature with the fixed frequency rate of
75.46 MHz.
2.3. Physical property analysis

2.3.1. Density measurement 2.6. X-Ray diffraction analysis (XRD)

The pycnometer setup is the standard protocol to assess the
density of the natural fibers [7]. A density known liquid toluene The crystallinity index of the FRRF was predicted with the help
was used to perform the density analysis (qtoluene = 866 kg/m3 at of XRD [24]. Crystallinity index is the measure of the degree of
room temperature). The collected FRRFs were placed in desiccators structural arrangement, whose measurement is so precious
which were packed with Silica gel for about 96 h in order to because which influences the mechanical properties. The investi-
remove the moisture contents presented in the fibers [15]. Then gation was carried out on X’PERT – PRO diffractometer. The oper-
the fibers were cut into 5 mm length small pieces for performing ating condition of the set up was set as V = 40 kV, I = 30 mA and
the density analysis test in the pycnometer. The mass of the pyc- k = 1.5406 Å. The X-Ray detector presented in the diffractometer
nometer was noted before (m1) and after (m2) filling up the FRRF. was used to scan the diffracted X-Ray between 10 and 80° (2h) at
The FRRF was then added with certain quantum of toluene whose 1° per min speed. The crystallinity index (CI) of FRRF was then cal-
mass value (m3) was already taken down. The final mass reading, culated by using Eq. (3) [20].
i.e., the mass of the mixed FRRF – toluene was measured (m4)   
Iamorphous
and noted. Then, the mass density of FRRF was examined using CI ¼ 1  100 ð3Þ
Icrystalline
the following relation (Equation (1)) [15].
where, Iamorphous – Intensity of the peak at the amorphous phase
ðm2  m1 Þ
qFRRF ¼  qtoluene ð1Þ (near 18° diffraction angle), and
ðm3  m1 Þðm4  m2 Þ
Icrystalline – Intensity of the peak at the crystalline phase (near
23° diffraction angle)
2.3.2. Diameter measurement
The diameter of the fiber has been predicted with the aid of The crystallite size (CS) was calculated by the Scherer’s formula
optical microscope. For that, twenty five distinct fiber samples as given below:
have been considered for the analysis; and from the microscopic
images taken along the longitudinal direction [5], the diameter of Kk
CS ¼ ð4Þ
the various fiber samples were noted and the average diameter b cos h
value has been considered as the nominal diameter of the FRR
where, K – Scherer’s constant, whose value is 0.89,
fiber.

k – Wavelength of the radiation,

2.4. Analysis of chemical composition b – the full width of the peak at the half-maximum, and
h – Bragg angle.
Distinct approaches were followed up for calculating the per-
centage of the chemical constituents such as cellulose, wax, hemi- 2.7. Thermal analysis
cellulose, moisture, lignin and ash content presented in FRRF. The
weight fraction of the cellulose content was evaluated based on 2.7.1. Thermogravimetric analysis
Krushner and Hoffer method. The rate of composition of hemicel- This analysis is a significant one for the study of thermal stabil-
lulose content was measured using neutral detergent fiber method ity of the constituents of the natural fiber decides the working tem-
[16]. The amount of lignin content was predicted with the aid of perature range of the composite materials prepared with such
APPITA P11s-78 approach [17]. Conrad method was used to mea- fibers [28]. Thermogravimetric analysis was carried out with Jupi-
sure the wax content [18]. The determination of ash content was ter Thermal Analyzer of STA 449 F3 model. FRRFs were crushed and
performed by finding out the weight difference between the 10 mg of the crushed fibers were taken in a platinum crucible and
burned and unburned FRRF [19]. In view of quantifying the amount kept into the thermal analyzer. Platinum crucible was used to
of moisture content in the fiber, the FRRFs were kept in an air oven avoid the variations in the temperature measurement using ther-
maintained at 80 °C nearly about 360 min. mocouple. The process was carried out in the 20 ml/min flow rate
nitrogen atmosphere in order to avoid oxidation. The samples were
2.4.1. FTIR analysis tested by increasing the temperature from 32 °C to 550 °C by
Fourier Transform Infrared (FTIR) analysis was conducted with increasing 10 °C/minute. The mass loss of FRRF during the test
the aid of the Perkin Elmer RXI spectrometer to characterize the was noted for every minute and the plot was drawn between the
various types and nature of chemical functional groups presented temperature in x- axis and % of weight loss in y- axis.
in the FRRF. For the Infrared measurement FRRF were crushed Broido’s equation (Eq. (2)) was used to predict the Kinetic Acti-
and mixed with Potassium Bromide (KBr) in the ratio of 1:100 vation Energy of FRRF.
due to the transparent behaviour of KBr. The prepared mixture       
1 Ea 1
was then compressed using a hydraulic pressure pellet maker for ln ln ¼ þK ð2Þ
y R T
1 min at 125 kg/cm2 pressure condition to form pellets of small
sizes. The spectrum was recorded in the range of 4000–500 cm1 Where, y – Normalized weight, i.e, Weight of the fiber at the
with 32 scans per minute and with the resolution of 4 cm1. considered time/ Initial weight,
 A. Arul Marcel Moshi et al. / International Journal of Biological Macromolecules 142 (2020) 212–221 215

Ea – Kinetic Activation Energy, Nanoscope IIIA, Veeco Co. Ltd., facilitated with a J- type piezo-
R – Universal Gas constant, electric scanner which had the tip radius of curvature of 10–
T – Temperature at the considered time (in K), and 20 nm [22]. The equipment used for getting the AFM micrographs
K – Constant of reaction rate. is capable of providing the results at 1 nm accuracy [25].

The minimum amount of energy needed to degrade the fiber

under consideration is termed as ‘kinetic activation energy’. 2.9. Tensile test on the proposed fiber

2.7.2. Differential Scanning calorimeter analysis The tensile test has been carried out using Universal Testing
This analysis has been performed with the help of Perkin Elmer Machine of INSTRON 5500R. The test was performed with the fiber
Pyrris 6 type Differential Scanning Calorimeter for supporting the samples of various gauge length values such as 10 mm, 20 mm,
thermogravimetric analysis results. For performing this analysis, 30 mm, 40 mm and 50 mm on the normal room temperature envi-
the fiber samples of 10 mg mass was placed inside aluminium pans ronment with 65% relative humidity. Twenty five samples were
and tightly sealed. Then the sealed aluminium pans containing the tested for each gauge length and their average value has been
fiber samples were kept inside the calorimeter and heated in the noted as the nominal tensile strength value of the fiber [5].
atmosphere of inert nitrogen gas from the room temperature upto
450 °C [25]. The melting peak values corresponding to the signifi- 3. Results and discussion
cant temperature (Tg) readings were taken at 10 °C/min heating
rate [23]. 3.1. Physical property analysis

2.8. Morphological study The mass density value of the FRRF was found to be 1246 kg/m3.
Density measurement was given equal importance to the mechan-
2.8.1. Scanning electron Microscopy ical property study since it highlights the natural fibers from syn-
Morphological study was carried out with a Scanning Electron thetic fibers [27]. The density of the proposed fiber is very nearest
Microscopy (SEM – VEGA3 TESCAN). The surfaces of FRRF were to that of the natural fibers obtained from Coccinia Grandis
pre-coated with a thin gold layer in order to avoid the unwanted (1243 ± 22.64 kg/m3) [15], Cissus Quadrangularis stem(1220 kg/
effects of the electron beam loading during testing. The morpho- m3) [5], Bagasse(1200 kg/m3)[5], Coir(1200 kg/m3) [5] and Jute
logical study of the gold pre-coated surfaces was performed with (1300 kg/m3) [5]. Because of the weight of the mass has direct
a 20 kilo Volt accelerating voltage and the results were obtained influence with the density, it needed to compare the density
with different enlargements. results of FRRF with other natural fibers; and, it was found that
the density of the proposed fiber was less than that of Lygeum Spar-
2.8.2. Energy dispersive X-Ray spectroscopy tum fiber(1499.7 ± 3.1 kg/m3) [2], Banana fiber(1350 kg/m3),
The presence of elements such as Carbon, Nitrogen, Oxygen, pineapple leaf fiber(1400 kg/m3), Sisal fiber(1500 kg/m3), Kenaf
etc., in the FRRR was examined using EDX (Energy Dispersive X- fiber(1310 kg/m3), Hemp fiber(1470 kg/m3), flax fiber(1500 kg/m3),
Ray Spectroscopy) of type INCAPentaFETx3, which is attached with Cotton fiber (1600 kg/m3) and Cissus Quadrangularis root fiber
the SEM. The distribution of the above said elements were noted at (1510 kg/m3) [5,13]. The main thing which was noted that the
five different locations on the fiber surfaces and their average val- measured density value of FRRF was very lower than the synthetic
ues were considered fibers like E-Glass fiber(2500 kg/m3), Carbon and aramid fibers
(1400 kg/m3)[5] which could be replaced by FRRF. The variation
2.8.3. Atomic force microscopic (AFM) analysis in the density value may occur due to several reasons, including
The Surface Roughness (Ra) profile was obtained and analysed environmental conditions and growth rate of the plant [2].The
with the help of an Atomic Force Microscope (AFM) of the model diameter value of FRRF in average was noted as 25.62 lm.

Table 1
Comparison table of chemical, physical and tensile properties of FRRF with other natural fibers.

Fiber Physical Properties Tensile properties Reference

Diameter (lm) 3
Density (kg/m ) Tensile Strength (MPa) Youngs Modulus (GPa) Strain to Failure (%)
Ficus Religiosa 25.62 1246 433.32 ± 44 5.42 ± 2.6 8.74 ± 1.8 –
Dichrostachys Cinerea – 1240 873 ± 14 – – [1]
Sida Rhombifolia – 1320.7 673 ± 14 – – [3]
Jute 40–350 1460 550 13 1.5 [5,6,12]
Flax – 1500 1100 100 2.4 [6]
Ramie 50 1500 8.0870 128 1.2 [6]
Hemp – 1480 690 70 1.6 [6]
Kenaf 65–71 1400 470–785 25.1 1.75–1.9 [5,12]
Sisal 50–300 1500 274–526 6.7–21.7 1.8–7.7 [5]
Cotton – 1600 200–400 5.5–12.6 7–8 [4]
Heteropogon Contortus – 602 476 ± 11.6 48 ± 2.8 1.63 ± 0.06 [4]
Cissus Quadrangularis stem 770–870 1220 4203 ± 1276 131 ± 37 4.78 ± 1.24 [5]
Cissus Quadrangularis root 610–725 1510 1875–5330 68–203 3.57–8.37 [5]
Artisdita hystrix – 540 440 ± 13.4 1.57 ± 0.04 – [15]
Ferula Communis 90–300 1240 475.6 52.7 – [15]
Althaea Officinalis L. 156–194 1180 415.2 65.4 3.9 [15]
Bamboo 240–330 910 503 35.91 1.4 [5]
Sea grass 5 1500 453–692 3.1–3.7 13–26.6 [5]
Alfa – 890 350 22 5.8 [5]
Coconut tree leaf sheath 140–990 1200 46.4 2.3 2.84 [5]
Piassava – 1400 134–143 1.07–4.59 7.8–21.9 [5]
216 A. Arul Marcel Moshi et al. / International Journal of Biological Macromolecules 142 (2020) 212–221

Table 2
Comparison table of chemical compositions of FRRF with other natural fibers.

Fiber Cellulose (Wt.%) Hemicellulose (Wt.%) Lignin (Wt.%) Wax (Wt.%) Moisture (Wt.%) Ash (Wt.%) Reference
Ficus Religiosa 55.58 13.86 10.13 0.72 9.33 4.86 –
Dichrostachys Cinerea 72.4 13.08 16.89 0.57 9.82 3.97 [1]
Sida Rhombifolia 75.09 15.43 7.48 0.49 12.02 4.07 [3]
Jute 72 13 13 0.5 12.6 0.5–2 [5,6]
Flax 81 14 3 1.7 10 – [6]
Ramie 76 15 1 – 8.0 – [6]
Hemp 74 18 4 2.3 10.8 – [6]
Kenaf 53.14 14.33 8.18 0.8 6.2–12 2–5 [5]
Sisal 60–78 10–14.2 8–14 2.0 10–22 – [5]
Cotton 82.7 5.7 – – 1.0 – [4]
Heteropogon Contortus 64.87 19.34 13.56 0.22 7.4 – [4]
Cissus Quadrangularis stem 82.73 7.96 11.27 0.18 – – [5]
Cissus Quadrangularis root 77.17 11.02 10.45 0.14 – – [5,13]
Artisdita hystrix 59.54 11.35 8.42 – – – [15]
Ferula Communis 53.3 8.5 1.4 – – – [15]
Althaea Officinalis L. 44.6 13.5 2.7 – – 2.3 [15]
Bamboo 26–43 30 1–31 – 9.16 – [5]
Sea grass 57 38 5 – – – [5]
Alfa 45.4 38.5 14.9 2 – – [5]
Coconut tree leaf sheath 27 14 27.7 – 4.7 – [5]
Piassava 28.6 25.8 45 – – – [5]

The comparison of the physical properties and tensile proper- FRRF are compared with that of few other natural fibers and pre-
ties of FRRF with another few raw natural fibers is presented in sented in Table 2.
Table 1.
3.3. FTIR analysis results
3.2. Analysis of chemical composition
The Fourier Transform Infrared spectra were observed between
Chemical composition analysis is essential to perform as a part the range of 4000 to 500 cm1, which is shown in the Fig. 2. The
of characterizing FRRF, because one can decide the mechanical maximum absorption peak was recorded at 3326 cm1, which
properties of a natural fiber with the aid of the wt.% of the contri- indicated the existence of hydroxyl (AOH) group present in the cel-
bution of each chemical composition. More amount of cellulose lulose contents [1,26]. The peaks occurred at 2922 and 2857 cm1
content ensures that the fiber has a high modulus of elasticity ensured the presence of wax contents (C„C stretching) distributed
and tensile strength [1,2]. FRRF has 55.58% cellulose content which with the fiber. The peak appeared at 1612 cm1 attributed the
is higher than that of kenaf (53.14%), Ferula Communis (53.3%), stretching of C@O group of hemicellulose contents [5]. The region
Althaea Officinalis L. (44.6%), Bamboo (26–43%), Alfa (45.4%), Wheat between 1439 and 1252 cm1 are associated with the C@H group
straw (51%), Coconut tree leaf sheath (27%), Piassava (28.6%), and of lignin contents [4]. The absorption peak appeared around
Kudzu (33%) [19], and nearer to that of Sea grass (57%), and Artisdita 1037 cm1 was occurred due to CAO and OAH stretching of
hystrix (59.54%). Higher the amount of hemicellulose has adverse polysaccharides in cellulose [8].
effect on the fiber strength [5]. The FRRF has 13.86% of hemicellu-
lose, which is lower than Sida Rhombifolia (15.43%), Flax (64.1– 13
3.4. C (CP-MAS) NMR spectroscopy
71.9%), Ramie (5–16.7%), Hemp (17.9–22.4), Heteropogon Contortus
(19.34%), Bamboo (30%), Sea Grass (38%), Alfa (38.5%), Wheat straw Fig. 3 shows the obtained NMR results for the FRRF. In the
(26%), Coconut tree leaf sheath (14%), Piassava (25.8%) and Kudzu obtained spectrum, the peak arrived at 63 ppm represents the
(11.6%) [19].
Higher levels of lignin help to retain water within the fiber,
which safeguards the fiber from biological attacks [1]; at the same
time, huge amount of lignin will cause for the deterioration of the
structure [5]. FRRF contains 10.13% of lignin, which is nominal. If a
natural fiber consists of the less weight fraction of wax content,
then the bond between the matrix and the fiber will be of higher
while fabricating composite structure with that fiber [1]. Flax
(1.7 wt%), Hemp(0.8 wt%), Kenaf(0.8 wt%), Sisal (2 wt%) and Alfa
fibers (2 wt%) have comparably higher wt.% of wax content than
FRRF which has 0.72 wt% of wax [19].
Fiber with low moisture content will have good bonding
between the fiber and polymer matrix of a composite material
[6]. Dichrostachys Cinerea fiber has almost the same amount of
moisture content (9.82%) of FRRF. FRRF holds 9.33% of moisture
content, which is lower than Sida Rhombifolia(12.02%),Jute(12.6%),
Flax(10%), Hemp(10.8%) and Sisal(10–22%). While the ash content
presented in a fiber, which will lead to the reduction of its amor-
phous phase.FRRF has 4.86% of ash content, which is higher than
Sida Rhombifolia(4.07%), Jute(0.5–2%), Kenaf(2–5%) [4] and Dichros-
tachys Cinerea (3.97%) [1]. The chemical composition details of the Fig. 2. FTIR spectrum for FRRF between the range of 4000–500 cm1.
 A. Arul Marcel Moshi et al. / International Journal of Biological Macromolecules 142 (2020) 212–221 217

crystallinity index was calculated as 42.92%. The crystallinity index

value of FRRF is higher than that of Juncus effuses (33.4%) [7], palm
fiber (19.9%) [7], Grewia tilifolia (41.7%) [6], Cyperus pangorei (41%)
[21] and untreated coconut fiber (29.93%) [7]. By means of alkali
treatment, the value of CI may get improved. The crystallite size
of FRRF was calculated with the aid of the Scherer’s formula, and
whose value is 5.18 nm. The crystalline and thermal properties of
FRRF are compared with that of other tested natural fibers and rep-
resented in Table 3.

3.6. Thermogravimetric analysis results

The thermal stability of the Ficus Religiosa natural fiber was

predicted with the help of Thermogravimetric Analysis (TGA), the
Derivative of the Thermogravimetric Analysis (DTG) graphs and
Broido’splot as shown in the Fig. 4(a)–(c). Normally, when a natural
fiber is exposed to high temperature conditions, the thermal degra-
dation occurs in the following order: hemicellulose, cellulose, lig-
Fig. 3. 13
C CP-MAS NMR spectra of FRRF. nin, wax and other constituents. From the Fig. 4(a), it is palpable
that the initial degradation peak was occurred at nearly 55 °C
amorphous nature of the cellulose contents (C6). The peak notable which indicated that the moisture contents present in FRRF got
near the 70–80 ppm range corresponds to the C2, C3 and C5 carbon evaporated at that temperature. Next degradation peak occurred
present in the cellulose contents. The presence of crystalline at 234 °C indicates the thermal degradation of hemicellulose con-
domain is ensured by the peak appeared between 80 and 85 ppm tents. The Cellulose contents got degraded at 325 °C temperature,
(C4). The peak near the 102.5 ppm spectrum is associated with which was noted by the steep curve present in the TGA and DTG
C1 (anomeric carbon) contents present in the fiber. The peaks pre- plots. The degradation peak occurred at 400 °C indicated the degra-
sent nearer to 174 ppm spectrum are attributed to COOH and CH3- dation of wax, lignin and other remaining constituents present in
COO chemical groups of hemicellulose constituents. The presence the FRRF. From the Broido’s plot, the kinetic activation energy
of aromatic carbon content corresponds to the lignin constituent was predicted as 68.02 kJ/mol.
is validated by the small and significant peaks occurred between
the spectra 108–170 ppm.
3.7. SEM (scanning electron microscope) results

3.5. XRD results Micro structural images were recorded using Scanning Electron
Microscope (SEM) with different magnifications for carrying out
The X-Ray diffractogram of FRRF is shown in Fig. 7. Two main the morphological study. This study holds significant importance
peaks were observed in the diffractogram corresponding to crystal- since the study provides the information that the fiber can be used
lographic planes (1 1 0) and (0 0 2). The crystallographic plane of as a suitable reinforcement agent for a particular composite applica-
(1 1 0) was noted at the diffraction angle 19.4° and the plane tion or not. It can be seen from the SEM image shown in Fig. 5 that
(0 0 2) was recorded at 2h = 24° diffraction angle [26]. The FRRF contains more amount of bounded hemicellulose and cellulose

Table 3
Comparison table of crystalline and thermal properties of FRRF with other natural fibers [15,16]

Fiber Crystalline Properties Thermal Properties

CI (%) CS (nm) Thermal stability (°C) Maximum degradation temperature (°C)
Ficus Religiosa 42.92 5.18 325 400
Dichrostachys Cinerea 57.82 – 226 495.3
Sida Rhombifolia 56.6 2.75 250 433.3
Jute 58.9 – 240 260
Flax 70 2.8 – –
Ramie 58 16 – –
Hemp 88 – 225 –
Sisal 75 – 250 275
Cotton – 5.5 265 280
Heteropogon Contortus 54.1 – 220 337.7
Cissus Quadrangularis stem 47.15 31.55 270 342.1
Cissus Quadrangularis root 56.6 28.05 230 328.9
Artisdita hystrix 44.85 – – 298.8
Ferula Communis 48 1.6 200 350
Althaea Officinalis L. 68 2.4 220 344
Juncus Effusus 33.4 3.6 200 300
Epipremnum Aureum 49.33 15 328.9 600
Perotis Indica 48.3 15 240 339.1
Red Banana Penduncle 62.1 12.1 230 353
Tridax Procumbens 34.46 25.04 195 330
Furcraea foetida 52.6 28.36 – –
Lygeum Spartum L. 46.19 – 220 338.7
218 A. Arul Marcel Moshi et al. / International Journal of Biological Macromolecules 142 (2020) 212–221

Fig. 4. (a) TGA&DTG (b) Broido plots (c) DSC curve of FRRF.

3.8. Energy dispersive X-Ray analysis (EDX)

Fig. 6 represents the amount of various elements distributed on

the surface of Ficus Religiosa fiber. The major peaks appeared on
the graph are Carbon, Oxygen, Sodium and Chlorin, which are the
major elements on the fiber surface. Among all the notable
elements, Carbon and Oxygen are the most dominant elements.
The weight and atomic percentages of all the observed elements
of FRRF along with that of few other natural fibers are presented
in Table 4.

3.9. AFM analysis results

The atomic force microscopic 2 dimensional and 3 dimensional

surface topographies are shown in Fig. 7. The average values of Ra
Fig. 5. SEM image of FRRF surface with 5X Magnification.
(Surface Roughness) and Rq (Root Mean Square Surface Roughness)
values of FRRF were predicted as 2.374 nm and 3.100 nm respec-
tively. This implied that the surface of FRRF was of partially rough,
contents, which could be reduced with the help of chemical treat- which is due to the existence of lignin, hemicellulose and wax
ments [6] in order to equip the fiber to get perfect bonding with contents present in the fiber. The surface skewness value of the
the matrix material while composite preparation [11]. fiber surface was found to be 1.540 [22], and the negative value
Porous parts were observed on the fiber surface. The observed of surface skewness indicated that the surface has porous sections
white layers in the SEM image are the hemicellulose contents. considerably [23]. The peak value obtained in the AFM micro-
Wax constituents also could be observed clearly from the image. graphs specifies the surface kurtosis, whose magnitude was noted
Also, the fiber surface is not so rough, which would reduce the fiber as 4.370, which specified that the surface of FRRF had smooth
– matrix adherence. Hence, modification is required in the fiber sections with the influence of wax like contents [23]. The Rz and
structure in order to achieve comparably good strength. Rt (Average Absolute Height Roughness and Maximum peak valley
 A. Arul Marcel Moshi et al. / International Journal of Biological Macromolecules 142 (2020) 212–221 219

Fig. 6. EDX Results of FRRF.

Table 4
Comparison of weight and atomic % of components present on the surface of FRRF with few other natural fibers.

S. No. Element FRRF Coccinia Grandis Cotton Jute

Weight % Atomic % Weight % Atomic % Weight % Atomic % Weight % Atomic %
1. C 67.48 75.50 44.67 51.91 46.1 53.2 55.68 62.72
2. O 25.32 21.27 54.38 47.58 53.9 46.8 43.89 37.11
3. Cl 3.11 1.18 0.38 0.06 0 0 0 0
4. Na 2.71 1.58 0 0 0 0 0 0
5. K 1.37 0.47 0 0 0 0 0 0
6. Al 0 0 0.18 0.09 0 0 0 0
7. Si 0 0 0.67 0.36 0 0 0.11 0.06
8. S 0 0 0 0 0 0 0.08 0.18

height) values usually tell us the nature of the surface, whose val-  The chemical composition analysis results provided the Cellu-
ues were marked as 13.901 nm and 23.077 nm respectively. Rz lose contents in the fiber as 55.58%, hemicellulose contents as
value is calculated by taking the difference between the maximum 13.86%, lignin contents as 10.13%, 0.72% wax contents, 9.33%
and minimum peak heights. Hence, higher value of Rz indicated moisture content and 4.86% of ash contents. The higher amount
that the fiber surface had smooth sections. of cellulose contents will yield good mechanical properties.
 SEM results indicated the wax contents, cellulose & hemicellu-
3.10. Single FRRF tensile test lose contents, porous and semi smooth surfaces of the FRRF.
 EDX results revealed that Carbon (67.48 wt%), Oxygen (25.32 wt
The average fiber diameter was determined from 25 samples %) and Chlorin (3.11 wt%) are the majorly participating
through optical microscope images taken in the longitudinal elements in the fiber structure.
direction using Image-pro software [5]. Table 5 shows that the  The thermal stability of the FRRF was predicted with the aid of
increase in gauge lengths from 10 mm to 50 mm, the tensile TG and DTG diagrams. Hemicellulose contents got degraded at
strength and Young’smodulus values also increases. As expected, 234 °C and cellulose contents at 325 °C. The kinetic activation
in FRRF natural fiber characterization the increases in thegauge energy was determined by means of Broido’s plot and whose
lengthobserved the minor deviationfrom the mean value for value was 68.02 kJ/mol.
various samples.  FTIR analysis ensured the chemical groups present with
cellulose (O@H), hemicellulose (C@O), lignin (C@H) and wax
4. Conclusions (C„C) contents.
 The crystallinity index value was calculated from the XRD
This study discussed the characterization of the novel natural analysis as 42.92% and whose value was found higher than that
fiber arrived from the root of Ficus Religiosa tree. The significant of Juncus effuses (33.4%), palm fiber (19.9%), Grewia tilifolia
outcomes from the study are listed beneath. (41.7%), Cyperus pangorei (41%) and untreated coconut fiber
(29.93%). The crystallite size was computed with the help of
 The density of FRRF was determined as 1246 kg/m3, which was Scherer’s formula as 5.18 nm.
compared with Lygeum Spartum fiber, Banana fiber, pineapple  The AFM micrographs helped to understand the nature of the
leaf fiber, Sisal fiber, Kenaf fiber, Hemp fiber, flax fiber, Jute fiber, fiber surface. The results justified that the fiber surface has
Cotton fiber and Cissus Quadrangularis root fiber. few porous parts and the surface is significantly smooth.
220 A. Arul Marcel Moshi et al. / International Journal of Biological Macromolecules 142 (2020) 212–221

Fig. 7. FRRF image acquired by AFM: Horizontal  3D (a) and 2D profile (b); Vertical  3D (c) and 2D (d) profile.

Table 5 [7] Mabrouk Maache, Abderrezak Bezazi, Salah Amroune, Fabrizio Scarpa, Alain
Tensile test results of FRRF. Dufresne, Characterization of a novel natural cellulosic fiber from Juncus
Effusus L, Carbohydr. Polym. 171 (2017) 163–172.
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Length (MPa) (GPa) % Extraction and characterization of natural cellulose fibers from maize tassel,
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20 mm 441.21 ± 24 5.37 ± 1.35 7.53 ± 1.7 Saravanakumar, M.R. Sanjay, Characterization of natural cellulosic fiber from
30 mm 447.37 ± 32 5.37 ± 1.21 8.06 ± 1.3 Epipremnum Aureum Stem, J. Nat. Fibers (2017).
40 mm 440.29 ± 28 5.24 ± 1.36 8.74 ± 1.5 [10] M. Prithivraj, R. Muralikannan, P. Senthamaraikannan, S.S. Saravanakumar,
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