Journal of Natural Fibers

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Effect of Alkalization on Characterization of

Ripe Bulrush (Typha Domingensis) Grass Fiber
Reinforced Epoxy Composites

M. Ramesh, C. Deepa, M. Tamil Selvan & K. Hemachandra Reddy

To cite this article: M. Ramesh, C. Deepa, M. Tamil Selvan & K. Hemachandra Reddy (2020):
Effect of Alkalization on Characterization of Ripe Bulrush (Typha�Domingensis) Grass Fiber
Reinforced Epoxy Composites, Journal of Natural Fibers, DOI: 10.1080/15440478.2020.1764443

To link to this article: https://doi.org/10.1080/15440478.2020.1764443

Published online: 20 May 2020.

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JOURNAL OF NATURAL FIBERS
https://doi.org/10.1080/15440478.2020.1764443

Effect of Alkalization on Characterization of Ripe Bulrush (Typha

Domingensis) Grass Fiber Reinforced Epoxy Composites
a
M. Ramesh , C. Deepab, M. Tamil Selvana, and K. Hemachandra Reddyc
a
Department of Mechanical Engineering, KIT-Kalaignarkarunanidhi Institute of Technology, Coimbatore, India;
b
Department of Computer Science and Engineering, KIT-Kalaignarkarunanidhi Institute of Technology, Coimbatore
Tamil Nadu, India; cDepartment of Mechanical Engineering, JNTU College of Engineering Anantapur,
Ananthapuramu, Andhra Pradesh, India

ABSTRACT KEYWORDS
Ripe Bulrush fibers (RBFs) is one of the grass fibers that have the potential Ripe Bulrush fibers; alkali
to replace synthetic fibers. This work focuses on the effect of alkalization on treatment; epoxy
characterization of Ripe Bulrush fiber-reinforced composites (RBRCs). The composites; fourier
composites are fabricated by compression molding process and the char- transform infra-red
spectroscopy; x-ray
acterization techniques such as Fourier transform infra-red (FTIR) spectro- diffraction; thermo-
scopy analysis, X-ray diffraction (XRD) studies, Differential scanning gravimetric analysis
calorimetry (DSC) analysis, Thermo-gravimetric analysis (TGA) and scanning
electron microscopy (SEM) studies have been carried out. From the results, 关键词
it is found that the significant improvement in properties and more thermal 成熟的芦苇纤维; 碱处理;
stability due to the alkalization. 环氧树脂复合材料; 傅里
叶变换红外光谱; X-射线
衍射; 热重量分析
摘要
成熟的灯芯草纤维(RBFs)是具有取代合成纤维潜力的草纤维之一. 研究了碱
化对成熟芦苇纤维增强复合材料性能的影响. 采用压缩成型工艺制备复合材
料，并采用傅立叶变换红外光谱分析、X-射线衍射、差示扫描量热分析、
热重分析和扫描电镜等表征技术对复合材料进行了表征. 结果表明，碱化处
理后材料的性能有了明显的改善，热稳定性有所提高.

Introduction
In recent years, the progress in the composite industry has led to the development of different fiber-
reinforced composite materials to obtain advanced material characteristics. Plant fiber-reinforced
composite materials is one of the ancient materials but the growth of these materials has developed
in the recent years. The advantages of plant fiber-reinforced composites are bio-degradable, eco-
friendly, recyclable, lightweight, low production cost, and readily available (Bhoopathi et al. 2015;
Ramesh, Palanikumar, and Reddy 2017). Therefore, these composites have been used for several
industrial applications such as making of automotive components, aerospace parts, sporting goods,
and building materials (Ramesh 2016). An alkali treatment was done to improve the interfacial
bonding between the fiber and matrix and thus obtaining better strength at the interface (Ramesh
et al. 2016). One of the plant fibers that has the potential to replace synthetic fibers is Typha fiber
(Baldwin and Angie 2007). Typha is a perennial plant and is an aquatic weed and it belongs to the
family Typhaceae in the plant kingdom (Su et al. 2019). This plant is mostly found throughout the
world and is widely grown in waterlogged areas and also in wastelands (Baldwin and Angie 2007;
Rizal, Huzni, and Thalib 2016).

CONTACT M. Ramesh mramesh97@gmail.com Department of Mechanical Engineering, KIT-Kalaignarkarunanidhi Institute

of Technology, Coimbatore-641402, Tamil Nadu, India.
© 2020 Taylor & Francis
2 M. RAMESH ET AL.

Fibers extracted from Typha plants have several advantages, such as good mechanical
properties, lightweight, low density, high tenacity, bio-degradability, etc. (Bawa et al. 2015;
Moghaddam et al. 2015; Ponnukrishnan, Thanu, and Richard 2014; Ramanaiah, Prasad, and
Reddy 2011; Wuzella et al. 2011). The wetted Typha leaves are twisted and wrapped around
the chair rungs to form a densely woven seat that is then stuffed. Many parts of the Typha
plant are edible to human beings. The starch which is called rhizomes extracted from this plant
are nutritious with protein content comparable to that of maize or rice (Morton 1975). The
seeds of this plant have a high content of linoleic acid and can be used to feed cattle and
chickens (Reed and Marsh 1955).
A study on the micro-mechanical bending behavior of Typha fiber composites was conducted
to investigate the interfacial adhesion between the fiber and matrix (Rizal, Huzni, and Thalib
2016). The result indicated that the epoxy resin distributed load to fiber immediately and Typha
fiber is capable of carrying the load properly. Ramanaiah, Prasad, and Reddy (2011) investigated
mechanical properties and thermal conductivity of Typha Angustifolia fiber reinforced polymer
composites. From the investigation, they concluded that tensile strength of composites increases
with increasing the fiber content. The similar result obtained by Ponnukrishnan, Thanu, and
Richard (2014) and they conducted experiment on the mechanical properties of Typha
Domingensis fiber-reinforced composites. Typha Angustata fibers were extracted and treated
with sodium hydroxide solution then the composites were fabricated with randomly oriented
fibers and the tests such as impact and hardness were conducted. The results showed that the
impact and hardness properties of the composite depend on the curing time of fibers in the
alkali solution (Kader, Sultana, and Khan 2019). Typha fibers were blended with polypropylene
matrix in order to investigate the effect of this reinforcement on the acoustic performance of
composites. The results revealed that the Typha fibers have good acoustic performance with
normal incidence absorption coefficient and claimed that these fibers could be a good choice for
sound absorption applications (Moghaddam et al. 2015).
Mechanical properties and thermal conductivity of Typha Angustifolia fiber composite were
measured. It is found that the mechanical properties are increased as increase in fiber content
and the thermal conductivity decreased when fiber content increased (Dedeepya, Raju, and
Kumar 2012). The chemical structure and crystallinity of Typha fiber composites were examined
via FTIR and XRD (Rizal et al. 2018). The tensile, flexural, and impact tests were also conducted
to investigate the effect of the alkali treatment on composite properties. From the tests, it is
found that the tensile, flexural, and impact strengths of the composites were increased after 5%
alkaline immersion when compared to untreated Typha fiber composites. Composite panels
manufactured from Typha leaves powder and the effect of binder content on compressive
strength and thermal properties have been investigated by Dieye et al. (2019). The results
showed that the compressive strength values obtained were comparable to the other plant
composite and reduction of the energy consumption as well as the emissions of carbon dioxide.
The thermal, rheological, and morphological properties of composites produced from Typha
plant stem powder were evaluated by Niang et al. (2018). It is found that the properties mainly
depend on the nature of the polymer and the Typha stem powder.
The valorization of Typha plant fiber as building material, the crushed fibers have been agglom-
erated using clay as binder. The influence of binder content on mechanical and thermal insulation
properties was examined. From the results, it is found that the compression and tensile strengths
respectively increase drastically when the weight percentage of binder is in the range of 77–85%
(Dieye et al. 2017). Diagne et al. (2005) found that the mechanical properties of composite materials
are improved by combining Typha, sisal pulp fibers, and polypropylene. Georgiev et al. (2014)
reported the test results of clay with Typha Latifolia fibers for their suitability as a plaster material.
From the literature, it is well known that few experimental studies have been done earlier on
mechanical properties; however, there is no report on characterization of alkali-treated RBRCs so
 JOURNAL OF NATURAL FIBERS 3

far. The objective of this study is to investigate the effect of alkali treatment on the characterization
of RBRCs.

Materials and methods

Materials
The materials used in this experimental study for composite fabrication are Ripe Bulrush (Family:
Typha Domingensis) fibers, epoxy resin, hardener, and Sodium hydroxide (NaOH) solution. The
Ripe Bulrush plants were harvested in the Cauvery river bank at Pallipalayam, Erode District, Tamil
Nadu, India. The epoxy resin (Type: LY556), hardener methyl ethyl ketone peroxide (MEKP) and
NaOH solution are purchased from M/s. Sakthi fiber glass Ltd., Chennai, Tamil Nadu, India.
Material properties of RBF and epoxy resin used for composite fabrication are presented in Table 1.

Methods
Fiber extraction
Ripe Bulrush is an herbaceous plant and its reproduction spreads rapidly by vegetative and generative in
tropical regions (Ashok Kumar et al. 2013). This plant is widely used in constructed wetlands for the
treatment of wastewater and contaminated soil and are helpful in some cases, where they can absorb
harmful chemical wastewater from industries (Nilratnisakorn, Thiravetyan, and Nakbanpote 2007). In this
experimental study, the combined retting process is used to extract the fibers from the leaves of the Ripe
Bulrush grass. In this process the plant is retted for 14 days and taken out then the fibers were extracted with
the help of the hand extraction machine manually. Then, the fibers were let to dry its moisture completely
for 3 days under the sunlight. The fibers length obtained is in the range from 1 to 42 cm. Then, the fibers are
treated with NaOH solution for 48 h to attain the fine surface and to improve the interfacial adhesion
between the fiber and the matrix. The Ripe Bulrush grass and the fibers extracted from them are presented in
Figure 1.

Fiber surface treatment

In order to improve the adhesion between the fiber and the matrix, the fibers have been subjected to
surface treatments (Ramesh et al. 2016). In the present experiment, the RBFs are treated with NaOH
solution (6% w/v) for 7 h at room temperature. Then, the surface-treated RBFs are washed with
deionized water, followed by the addition of 0.1 N hydrochloric acid to remove the impurities.
Finally, the fibers are dried in an air circulated oven at 60°C for 24 h.

Fabrication of composites
In this experimental study, the composite used for characterization is fabricated by compression
molding process. The RBFs are randomly oriented and the composites have been fabricated. A thin

Table 1. Properties of RBF and epoxy resin (Joao 2012; Moghaddam et al.
2015; Mortazavi and Meghdad 2009; Ramesh, Sudharsan, and Palanikumar 2015;
Witztum and Randy 2014).
Property RBF Epoxy resin
Density (g/cm3) 1.25 ± 0.1 1.16
Tensile Strength (MPa) 202 73
Young’s Modulus (MPa) 11.56 5
Fiber length (mm) 80 ± 5.7 -
Fiber diameter (μm) 66.7 ± 12 -
Fiber fineness (Tex) 4.4 ± 0.3 -
Breaking elongation (%) 1.7 ± 0.2 0.8-6
Tenacity (cN/Tex) 30.0 ± 6.5 40.5 ± 3.4
Toughness (MJ/m3) - 100-200
4 M. RAMESH ET AL.

Figure 1. Ripe Bulrush grass and extracted fibers.

Figure 2. Fabricated composite laminate.

polyethylene sheet is spread over the wooden mold and silicon spray is applied on the sheet for easy
removal of the fabricated composite laminate. The fibers are cut into 25 mm length and distributed
uniformly at the bottom of the mold which is prepared earlier. The resin is poured over the fiber
layer in an evenly manner and left curing for 5 h. A load of 10 metric tons was applied on the plates
by using hydraulic compression machine to form a uniform laminate. The fabricated composite
laminate is presented in Figure 2.

Experimentation
In this experimental study, the RBRCs have been fabricated by compression molding process. The
characterization techniques such as FTIR spectroscopy, XRD, DSC, TGA, and SEM studies have
been carried out. The types of the samples used for various tests are given in Table 2.
 JOURNAL OF NATURAL FIBERS 5

Table 2. Sample types for various tests.

Test No. Name of the test Sample type
1 TGA Powder
2 FTIR Powder
3 DSC Powder
4 XRD Plate
5 SEM Plate

FTIR spectroscopy
FTIR spectroscopy studies have been carried out to identify the chemical structure and the changes
in the structure of fibers and polymers (Saba et al. 2019). FTIR spectroscopy is an effective technique
that is used to analyze the organic compounds in the material. Infra-red spectra of samples were
recorded using an FTIR spectrometer (Model: Perkin-Elmer). The sample was cooled and powdered
then diluted to 1% using potassium bromide (KBr), and pellets were prepared by using a ball mill.
The FTIR spectra of the composite samples were recorded in the 4000–400 cm−1 region with 32
scans in each case at a resolution of 4 cm−1.

Thermo-gravimetric analysis
TGA test is conducted to analyze the change in mass while increase in temperature. A change in
thermal stability was examined in terms of percentage weight loss as a function of temperature is
estimated in this method. The mass change characteristics of a material were strongly dependent on
the typical experimental conditions, pressure of the atmosphere in the sample chamber, and the
scanning rate have vital influences on the characteristics of the recorded curve (Reddy et al. 2019). In
this experiment, the thermo-grams of the RBRC sample were recorded by using an instrument
(Model: Perkin Elmer 4000 series) in nitrogen atmosphere at a heating rate of 10°C/min.

Differential scanning calorimetry analysis

DSC is used to analyze the thermal transitions of surface-modified RBRCs. Samples were subjected
to a temperature scanning ranging from 30°C to 500°C, at a heating rate of 10°C/min under a flow of
nitrogen gas. In this experimental study, we performed heating-cooling cycles under controlled
atmosphere during the temperature programming. The processing and the residual stresses in
materials of thermal origin were eliminated during the heating cycle. Then, the cooling cycle
made it possible to measure the melting temperature, the melting enthalpy, the crystallinity degree
of semi-crystalline polymers and the heat capacity variation of the composites. In this experiment,
DSC experiments have been carried out by using calorimeter of type Perkin Elmer Pyris 1.

X-ray diffraction studies

XRD is taken to analyze the chemical composition and crystalline structure of the composites. The
phase changes in modified RBFs in terms of crystallinity can be analyzed by this technique. The XRD
experiments were performed using a diffractometer (Model: Rigaku Dmax 2500). The setup has
a rotating anode generator with a copper target and a powder goniometer. The generator was
operated at 40 kV and 150 mA. All the experiments were performed in the reflection mode at a scan
speed of 4°/min in steps of 0.05.
6 M. RAMESH ET AL.

Scanning electron microscopy analysis

The SEM study is conducted to analyze the fiber surface texture, internal bonding of fiber, and
matrix of RBRC samples. SEM micrographs of the fabric after alkali-treatment were recorded using
an electron microscope (Model: JEOL TM 3030). The samples were gold coated before scanning the
micrograms.

Results and discussion

In this experimental study, the composite laminates were fabricated by reinforcing the alkali-treated
RBFs by using compression molding process. The samples were prepared according to ASTM
standards. The characterization techniques such as FTIR spectroscopy, XRD, DSC, TGA, and SEM
studies have been carried out and the results are discussed in this section.

Differential scanning calorimetry analysis

The DSC, which is known to be one of the popular technique used to determine various thermal
parameters such as heat flow rate and curing behavior (Saba et al. 2019). The effect of alkali-
treatment on the curing behavior of the RBRCs is studied in this analysis. The analysis is performed
by using a DSC machine by taking 2–3 g of RBF powder is placed and sealed in aluminum pan at the
heating rate of 10°C/min. The DSC curve is presented in Figure 3. The endothermic peak was
observed in the temperature range of 250-480°C and may be attributed to the loss of moisture from
the RBFs. The peaks seen in the DSC profile are in good agreement with the mass loss seen in this
temperature range of fiber (Madhu et al. 2019).

Thermo-gravimetric analysis
TGA measures the amount of weight change of a material, either as a function of increasing
temperature, or iso-thermally as a function of time, in a nitrogen atmosphere. This is the widely
used technique to evaluate thermal properties and kinetics of reaction. The weight change pattern of

Figure 3. DSC analysis of the composites.

 JOURNAL OF NATURAL FIBERS 7

Figure 4. Thermo-gram of RBRCs.

a composite material is strongly dependent on the experimental conditions such as weight of the
sample, volume and physical structure, shape and position of the specimen holder, and atmospheric
pressure inside the chamber and the scanning rate, etc. In this experimental study, TGA was
performed to categorize the effect of alkali-treatment on the thermal stability RBRCs. The results
of TGA analysis are presented in Figure 4. From the figure, it has been suggested that the NaOH
treated RBRCs exhibit remarkable thermal behavior through TGA studies. It is found that upto 280°
C there is no big change in the thermal stability of the composites start losing weight at 300°C and
lost almost its entire weight at 400°C.
Also, found that the further weight losses in the temperature range between 300°C-400°C due to
degradation of cellulose, hemicelluloses, lignin, pectin, and chemical cross link of various cellulose
matters of RBFs. Researchers explored this is due to eco-friendliness violation in amorphous
hemicelluloses and lignin during alkali treatment (Jayaramudu, Guduri, and Rajulu 2009; Reddy
et al. 2019). This is the evidence that the RBRCs have higher thermal stabilities at initial stage. From
the literature, we came to know that the alkali-treated plant fibers exhibit higher degradation
temperature when compared to the untreated one (Sanjay et al. 2018). This result is reflected in
our experimental study.

FTIR analysis
FTIR analysis or spectroscopy is an analytical technique that is used to identify organic, polymeric,
and, in some cases, inorganic materials. The FTIR analysis method uses infra-red light to scan test
samples and observe chemical properties. The alkali-treatment is used to remove the hemi-
cellulose and lignin from the fiber surface, which increases the amount of cellulose on the fiber
surface, thereby increasing the bond strength as well as the number of reaction sites (Aboul-Fadl
et al. 1985). The results of the FTIR analysis are presented in Figure 5. The absorbance peaks have
been identified in the region 3332–2919 cm−1 is attributed to the characteristic of the hydroxyl
groups. The two peaks observed at 1507 and 1361 cm−1 are ascribed to C = O stretching of the
8 M. RAMESH ET AL.

Figure 5. FTIR analysis of the composites.

amide group presented in hemicellulose and lignin, respectively. A noticeable peak at 826 cm−1 is
attributed to C-OH stretching of lignin and confirms that the surface modification helps in
eliminating hydroxyl and carboxyl groups from the fibers, thereby making them have good
interfacial adhesion.

X-Ray diffraction analysis

XRD is an analytical technique mainly used for phase identification of a crystalline material and can
provide information on unit cell dimensions. The analyzed material is finely ground, homogenized,

Figure 6. XRD results of the composites.

 JOURNAL OF NATURAL FIBERS 9

Table 3. Crystal structures of the components.

Score Compound name Chemical formula Crystal structure
53 Cadmium Aluminum Cd4Al2O6(SO4)14H2O Hexagonal
Oxide Sulfate Hydrate
52 Sodium Borane Na2(H12B12) Monoclinic
47 Aluminum Phosphate Al2PO4SiO6 Unknown
Silicate

and average bulk composition TGA is determined. The results of XRD analysis are presented in
Figure 6. From the figure, it can be observed that the results exhibited non-crystalline material
presence; it shows the crystallinity depends on the fiber content reinforced in the material.
Therefore, the crystallinity increased with an increase in fiber wt. % due to alkali-treatment. The
components and their crystal structures are given in Table 3.

SEM analysis
SEM provides detailed high-resolution images of the sample by rastering a focussed electron beam
across the surface and detecting secondary or backscattered electron signal. SEM provides images with
magnifications well beyond the range of optical microscopes. The alkali-treated fibers reinforced
composites had higher storage moduli than the un-treated one, which indicated good bonding between
the fibers and the resin (Ramesh 2019). The internal structure of Typha leaves has been explained by
several researchers (Kaul 1974; McManus, Seago, and Marsh 2002; Meyer 1933; Rowlatt and Morshead
1992; Teale 1949). The SEM images of the RBRC samples are presented in Figure 7. The magnified view
of the alkali-treated RBF surface is presented in Figure 7(a). From the image, it is clearly observed that
the fiber is not exactly not circular in the cross-section and the presence of unwanted particles inside the
fabricated composite laminate. The surface decomposition of the fiber due to NaOH solution concen-
tration is shown in Figure 7(b). From this image, it is clearly seen that the fibers appear to be present
mainly as ultimates and well-separated from the matrix.
The surface of the fabricated composite laminate is presented in Figure 7c. The resin distribution
on the surface of the laminate is clearly visible from this image. The fiber orientation inside the
composite laminate is shown in Figure 7d. This image clearly showed that loosely bonded fibers and
poor interfacial adhesion between them; also, the gap between the fiber and matrix layer can be
clearly identified. The image presented in Figure 7e further shows that the visibility of clean fiber
surface indicating poor wettability of fibers and weak bonding. The nature of fiber fracture of the
tested composite sample is presented in Figure 7e. From the image, it is known that the fiber fracture
takes place along the direction of load applied and depends on the fiber orientation in the laminate.
It also shows the effect of loading on the composite material and able to see the fiber breakage caused
by the applied load toward the material. The structure of the RBF is almost similar to the result
obtained by Witztum and Randy (2014).

Conclusion
In this experimental study, Ripe Bulrush grass leaf fiber is used as a reinforcing material for the
development of new composites. The epoxy resin is used to fabricate the composites by compression
molding process and the characterization techniques such as FTIR spectroscopy, XRD, DSC, TGA,
and SEM studies have been carried out. The conclusion of this experimental study is as follows:

● The results showed that the epoxy resin distributed load to fiber immediately and RBF is
capable of carrying the load properly.
10 M. RAMESH ET AL.

Figure 7. SEM images of (a) RBF, (b) alkali-treated fiber surface, (c) composite laminate surface, (d) fiber orientation inside the
composite laminate, and (e) fractured fiber.

● The endothermic peak was observed in the temperature range of 250-480°C which is identified
from the DSC analysis. This peak showed that the reduced catalytic effect on fibers due to
alkali-treatment of fibers.
● RBRCs exhibit remarkable thermal behavior and found that upto 280°C there is no big change
in the thermal stability of the composites and start losing weight at 300°C found from TGA
studies. It is proved that the decomposition temperature and thermal stability of the alkali-
treated RBRCs are high.
 JOURNAL OF NATURAL FIBERS 11

● The absorbance peaks have been identified in the region 3332–2919 cm−1 is attributed to the
characteristic of the hydroxyl groups. This study confirmed that the diversified applications of
RBRCs.
● From the XRD studies, it is found that the crystallinity depends on the fiber content reinforced
in the composites.
● From the XRD and SEM studies, it is found that an increase in crystallinity due to alkali-
treatment of RBFs.
● The results of this study showed that the composites reinforced with RBFs could be considered
as relatively acceptable alternatives for synthetic fibers, because of their excellent properties.

ORCID
M. Ramesh http://orcid.org/0000-0002-8401-2521

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