Journal of Natural Fibers
ISSN: 1544-0478 (Print) 1544-046X (Online) Journal homepage: https://www.tandfonline.com/loi/wjnf20
Natural Cellulosic Fiber from Coccinia Indica
Stem for Polymer Composites: Extraction and
Characterization
Mylsamy Bhuvaneshwaran, Sampath Pavayee Subramani, Sathish Kumar
Palaniappan, Samir Kumar Pal & Sethuraman Balu
To cite this article: Mylsamy Bhuvaneshwaran, Sampath Pavayee Subramani, Sathish Kumar
Palaniappan, Samir Kumar Pal & Sethuraman Balu (2019): Natural Cellulosic Fiber from Coccinia
Indica Stem for Polymer Composites: Extraction and Characterization, Journal of Natural Fibers,
DOI: 10.1080/15440478.2019.1642826
To link to this article: https://doi.org/10.1080/15440478.2019.1642826
Published online: 23 Jul 2019.
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JOURNAL OF NATURAL FIBERS
https://doi.org/10.1080/15440478.2019.1642826
Natural Cellulosic Fiber from Coccinia Indica Stem for Polymer
Composites: Extraction and Characterization
Mylsamy Bhuvaneshwarana, Sampath Pavayee Subramanib, Sathish Kumar Palaniappan c
,
Samir Kumar Palc, and Sethuraman Balud
a
Department of Mechanical Engineering, K. S. R. College of Engineering, Tiruchengode, Tamil Nadu, India;
b
Department of Mechanical Engineering, K. S. Rangasamy College of Technology, Tiruchengode, Tamil Nadu, India;
c
Department of Mining Engineering, Indian Institute of Technology Kharagpur, Kharagpur, West Bengal, India;
d
Department of Mechanical Engineering, PSNA College of Engineering and Technology, Dindigul, Tamil Nadu, India
ABSTRACT KEYWORDS
This study mainly focuses on the possibility of using Coccinia Indica (CI) fiber as Coccinia Indica fiber;
reinforcement in structural polymer composite materials because of its light- technical properties;
weight and eco-friendly nature. Fibers were extracted from the dried stems by morphology; reinforcement;
combing process using metal teeth brush. The thermo-physico-mechanical conventional fibers;
medicinal plant
properties, chemical compositions, and morphological structures of CI fiber
were analyzed in detail. A higher percentage of cellulose content in CI fiber 关键词
and the lesser amount of skimpy lignin, hemicellulose, ash, and wax content were 胭脂虫纤维; 技术性能; 形
confirmed through chemical analysis. The functional groups with their corre- 态强化; 传统纤维; 药用植
sponding peaks were depicted through FTIR analysis. XRD studies divulge that 物
the CI fiber contains crystallinity index (CrI) of 53.03% and crystallite size (L) of
5.81 nm. SEM revealed that the fiber possesses cylindrical morphology with
multi-cellular structure. The presence of parenchyma and chlorenchyma tissues
in the cell wall of CI fiber was also confirmed, which helps for better adhesion and
mechanical properties to the composite. TGA study reveals that the major
degradation of CI fiber occurs at a temperature range of 204.16°C to 376.3°C.
The tensile strength of cellulose-based CI fiber is comparable with the other
conventional fibers and it is well enough for its usage as reinforcing material in
composite manufacturing.
摘要
本研究主要探讨了球虫夏草纤维（CI）以其轻质、环保的特性在高分子结
构复合材料中作为增强材料的可能性.采用金属牙刷梳理法从干燥的茎中
提取纤维.详细分析了CI纤维的热物理力学性能、化学成分和形态结构.化
学分析证实，CI纤维中纤维素含量较高，而脱脂木质素、半纤维素、灰分
和蜡含量较低.通过FTIR分析，描述了各官能团的相应峰。XRD研究表明，
CI纤维的结晶度指数（CRI）为53.03%，结晶尺寸（L）为5.81nm.扫描电
镜分析表明，纤维具有多胞结构的圆柱形结构.同时证实了CI纤维细胞壁
中存在薄壁组织和厚壁组织，有助于提高复合材料的粘附力和力学性能.
TGA研究表明，CI纤维的主要降解发生在204.16°C至376.3°C的温度范围内.
纤维素基CI纤维的拉伸强度与其他常规纤维相当，足以作为复合材料制造
中的增强材料.
Introduction
Currently, researchers mainly focused on the biodegradable material, i.e., natural fiber in the
composite fabrication which will have vast advantages like more innocuous, recyclable, cheap and
CONTACT Sathish Kumar Palaniappan sathishiitkgp@gmail.com Department of Mining Engineering, Indian Institute of
Technology Kharagpur, Kharagpur, West Bengal 721 302, India
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/wjnf.
© 2019 Taylor & Francis
2 M. BHUVANESHWARAN ET AL.
absence of health risks. In contrast to conventional reinforcement materials, cellulose-based fibers
were used as reinforcement elements in bio-composites, because of its advantages such as low cost,
low density, acceptable specific strength and good thermal properties (Thakur, Thakur, and Gupta
2014; Harish et al. 2009). Maturity of the plant and process implemented for its extraction
determines its mechanical properties (Mohanty, Misra, and Drzal 2001). Hence, researchers pay
their attention towards natural fiber with demonstration potential for reinforcement either with
thermo-set or thermo-plastic matrix, coir (Dicker et al. 2014), sisal (Li, Mai, and Ye 2000; Oksman
et al. 2002), flax (Goutianos et al. 2006) (Hornsby, Hinrichsen, and Tarverdi 1997; Yan, Chouw, and
Jayaraman 2014; Zhu et al. 2013), jute (Ahmed and Vijayarangan 2007; Mohanty and Misra 1995;
Sever et al. 2012) and hemp (Madsen et al. 2007; Shahzad 2011). Identification of natural fiber is
turned into a challenge for researches in bio-composite material community, because the ranges of
those fibers are narrow. For example, from the past five years, cellulose-based fibers such as cissus
quadrangularis root fiber (CQRF) (Indran, Raj, and Sreenivasan 2014), manicaria saccifera (Porras,
Maranon, and Ashcroft 2015), arundo donax (Fiore, Scalici, and Valenza 2014), ferula communis
(Seki et al. 2013), sansevieria ehrenbergii (Sathishkumar et al. 2013), polyalthia cerasoides
(Jayaramudu et al. 2009) and calotropis gigantea (Ganeshan et al. 2018) have been recommended
as remarkable alternatives to reinforce novel composites. Urtica dioica natural fiber was investigated
and reported that it can be used to fabricate eco-friendly natural fiber-reinforced composite (Bodros
and Baley 2008). Composites are extensively used in the automobile industries (Thakur, Thakur, and
Gupta 2014). A fabricated household telephone stand that uses a natural banana fiber and epoxy
resin was found to be eco-friendly and the same will also be utilized for developing low-cost
household appliances (Sapuan and Maleque 2005). It is inferred from the recent literatures that
the natural fiber composites play a vital role and the low-density natural fibers have been used to
manufacture lightweight composites. In this investigation, an attempt is made in this paper to study
the thermo-physico-mechanical properties and morphology characterizations of the Coccinia Indica
(CI) fiber and introduce them as novel natural reinforcement to the composites.
Materials and experiments
Extraction of fiber
The matured CI plants were collected from Kanuvukarai Village, Coimbatore District, Tamil Nadu
State, India, which is a medicinal plant under the family of Cucurbitaceae (Ajithabai et al. 2011; Ali
et al. 2008; Sivasankari, Anandharaj, and Gunasekaran 2014). Figure 1 shows the CI stems and
extracted fibers after the microbial degradation process. In this process, fibers were separated from
the CI plant stem and it was dipped into the water for 3 weeks to allow for microbial degradation.
Then, the soaked stems were cleaned with freshwater and dried in the open atmosphere for a week.
Figure 1. Fiber extraction process (a) sliced CI stems immersed in water (b) CI stems in water after 3 weeks (c) extracted fibers.
JOURNAL OF NATURAL FIBERS 3
Finally, the fibers were extracted from the dried stems by combing process with the metal teeth
brush.
Chemical–physical property analysis
To compute the maximum tensile strength of the single fiber, tensile tests were carried out on the
extracted fiber prepared as per ASTM D3822 M14 standard. INSTRON 5500R tensile testing
machine with the aid of 1 kN load cell was employed in this study. During testing, 50 mm gauge
length specimen was subjected to a crosshead speed of 5 mm/min, and the entire test was performed
under room temperature. The chemical analysis was done to determine the content of cellulose,
lignin, wax, moisture, and density as per the standards (Boopathi, Sampath, and Mylsamy 2012).
Fourier transform infrared (FTIR) analysis
To figure out the functional groups in CI fiber, Fourier Transform Infrared (FTIR) analysis was
carried out using Perkin Elmer RXI FTIR tester with the scanning rate of 30 scans per minute at
a resolution of 5 cm−1 in the wavenumber region of 500–4000 cm−1. The fine powder was prepared
using ball miller from the chopped samples and then mixed with KBr. Then, the powder was
pelletized by applying pressure to prepare the specimen for FTIR spectra under standard conditions.
X-ray diffraction (XRD) analysis
The crystallinity index (CrI) of CI fiber was calculated using powder X-Ray Diffraction (XRD)
method with the help of X’PERT PRO diffractometer. The parameters used in XRD analysis are
monochromatic Cu-Kα radiation with the wavelength of 0.154 nm, current of 30 mA, copper anode
and the signal absorption ranges between 10°C and 80°C.
Thermogravimetric-difference thermogravimetric (TG-DTG) analysis
Thermogravimetric (TG) and Difference Thermogravimetric (DTG) analysis was performed on the
CI fiber samples using Jupiter Simultaneous Thermal Analyzer (Model STA, NETZSCH). Nitrogen
inert gas was used to avoid the oxidation of samples during testing. The sample was kept on the
ceramic crucible to establish proper contact between the thermocouple and CI fiber samples. The
heating rate of 10°C/min over a range of 30–600°C was utilized in this experiment.
Scanning electron microscopy (SEM) analysis
Scanning Electron Microscopy (SEM) analysis was carried out to reveal the surface morphology of
the CI fiber. SEM analysis was carried out using the CARL ZEISS model V18. Gold sputtering was
done on the surface of samples before SEM analysis to avoid electrical charge accumulation.
Results and discussions
Chemical–physical property analysis
The chemical analysis was performed on the CI fiber and the results are tabulated in Table 1.
Generally, the presence of cellulose and lignin content offers good tensile property and rigidity to the
fiber, respectively. In this study, the tested CI fiber contains high cellulose and lignin contents with
low wax and ash contents. Especially, the cellulose percentage makes an impact on mechanical
properties of the fiber (Indran, Raj, and Sreenivasan 2014). Mechanical properties were determined
from randomly selected 20 samples of a given bundle of fibers, and the average tensile strength
4 M. BHUVANESHWARAN ET AL.
Table 1. Chemical-physical properties of the CI fiber in comparison with other cellulose-based natural fibers.
Hemi- Tensile
Cellulose cellulose Lignin Wax Moisture Density (kg/ Elongation strength
Fiber (%) (%) (%) (%) (%) m3) (%) (MPa) Ref.
CI 64.56 14.09 12.55 0.25 7.27 1370 4.46 645 Present
work
CQRF 77.17 11.02 10.45 0.14 7.30 1510 3.57–8.37 1857–5330 [16]
Arundo Donax 43.20 20.50 17.20 - - 1168 3.24 248 [18]
Ferula Communis 53.30 8.50 1.40 - - - 4.20 476 [19]
Sansevieria 80.00 11.25 7.80 0.45 10.55 887 2.80–21.70 50–585 [20]
Ehrenbergii
Polyalthia 64.50 22.70 12.60 - - - 2.50 44 [21]
Cerasoides
values are also tabulated in Table 1. Chemical and physical properties of the CI fiber were compared
with other natural fibers, and it clearly depicts that tensile strength of the cellulose-based CI fiber is
enough for its usage as reinforcing material in composite manufacturing.
FTIR analysis
The FTIR analysis to determine the functional groups present in the CIF was conducted on the
prepared samples and the results are presented in Figure 2 and Table 2.
XRD analysis
The XRD result depicts in Figure 3 inferred that the couple of well-defined peaks could be observed.
The peak at 2θ = 22.37° (200) clearly indicates the cellulose content and the peak at 2θ = 15.66° (100)
shows the typical non-cellulose materials which could be lignin, wax, etc. Commonly, CrI was used
Figure 2. FTIR spectrum of CI fiber.
JOURNAL OF NATURAL FIBERS 5
Table 2. Functional groups and their corresponding peaks (cm−1) of CI fiber.
Bond/stretching CI fiber peak (cm−1) Assigned functional groups Ref.
O-H 3356 Presence of cellulose [16]
C-H 2924 Vibration of cellulose [29]
C=O 1735 Hemicellulose [17]
C=C 1654 Lignin, calcium pectates and water [30]
C-O 1236 Cellulose and hemicellulose [31]
C-O-C 1031 Modes of hydroxyl and cellulose [32]
C-OH 897 Bending in cellulose [33]
Figure 3. XRD spectrum of CI fiber.
to measure the crystalline of cellulose with respect to the amorphous materials. The following
expression was employed to compute the CrI (Segal et al. 1959) of CI fiber.
ðI002 IAM Þ
CrI ¼ 100 (1)
I002
CrI denotes the relative degree of the crystallinity, I002 refers the maximum intensity, and IAM
represents the minimum intensity. CrI of the CI fiber was found to be 53.03%. The crystallite size (L)
of CI fiber was determined by Scherer’s equations (Park et al. 2010) and it was found to be 5.81 nm.
kλ
L¼ (2)
βcosθ
6 M. BHUVANESHWARAN ET AL.
where k is Scherer’s constant (0.94), β is the peak’s FWHM (field width at half maximum) and λ is
the wavelength of the radiation.
TG-DTG analysis
Thermal characteristics of the CI fiber were studied using TG and DTG curves obtained from the
thermogravimetry analysis as shown in Figure 4. It is inferred from the figure that the degradation of
CI fiber occurred in different stages. The first stage (up to 69.16°C) shows the loss of moisture and
a mass change was found to be 9.1% as predicted (Moran et al. 2008). Similarly, mass change of
19.26% was found at next peak shown from 69.16°C to 204.16°C, where pyrolysis of lignin is
initiated (French 2014). The third stage (between 204.16°C and 376.3°C) is the degradation of
cellulose and part of lignin with the mass change of 51.02% (Silverio et al. 2013), similar peaks
were observed at 321°C, 309.2°C, and 308.2°C for bamboo, kenaf, and hemp fibers, respectively (Yao
et al. 2008). The reason for major mass change in the third stage is due to the degradation of
cellulose which is higher in the CI fiber. In this stage, the chemical analysis shows the higher amount
of cellulose in the temperature above 376.3°C is due to breaking of aromatic structure present in the
lignin, dehydration and methane gas release were taking place simultaneously. In the final stage, the
temperature ranges above 376.3°C, the degradation of part of cellulose and lignin occurs and the
mass change was observed to be 7.52%.
Figure 4. TG/DTG curves of CI fiber.
JOURNAL OF NATURAL FIBERS 7
Figure 5. SEM images of single CI fiber at a magnification of (a) 10 µm and (b) 200 µm.
SEM analysis
It is inferred from Figure 5(a) that the CI fiber possesses a multi-cellular structure with a diameter of
15 μm approximately. Moreover, from Figure 5(b), it is observed that the CI fiber is soft in nature
and looks like a cylindrical shape with a diameter of 390 μm approximately. The cylindrical
morphology in the natural fiber increases the specific area and thus favors the chemical processes.
Similarly, it is observed from Figure 5(b) that the functional groups of parenchyma and chlorench-
yma tissues were present in the cell wall of the CI fiber plant stem which offers better adhesion and
mechanical properties to the composite.
Conclusion
Investigation on the thermo-physico-mechanical properties, chemical compositions and morpholo-
gical structures of CI fiber was presented to evaluate the possibility of using them as reinforcement in
polymer composite materials. The chemical analysis and spectral analysis results showed that the
higher percentage of cellulose content (64.56 wt.%) was present in the CI fiber and the rest includes
lignin, hemicellulose, wax, and moisture. The mechanical properties with a crystalline index of
53.03% and a crystallite size of 5.81 nm are comparable with the other conventional fibers. The
thermal analysis results indicate that the CI fiber is stable up to 204.16°C, which is higher than the
polymerization process temperature. The density of CI fiber is significantly lower (1.37 g/cm3) in
comparison with synthetic fibers such as E-glass fiber (2.5 g/cm3). Therefore, CI fiber could be used
as a reinforcement material in structural polymer composites because of being lightweight and eco-
friendly.
Acknowledgments
The authors are thankful to LMP R&D Laboratory, Erode, Tamil Nadu State, India and PSG College of Technology,
Coimbatore, Tamil Nadu State, India for providing their facilities for testing the samples.
ORCID
Sathish Kumar Palaniappan http://orcid.org/0000-0002-2227-6433
8 M. BHUVANESHWARAN ET AL.
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