Journal of Natural Fibers

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Effect of Green Gram Husk Nanocellulose on

Banana Fiber Composite

Mounika Movva & Ravindra Kommineni

To cite this article: Mounika Movva & Ravindra Kommineni (2017): Effect of Green
Gram Husk Nanocellulose on Banana Fiber Composite, Journal of Natural Fibers, DOI:
10.1080/15440478.2017.1414658

To link to this article: https://doi.org/10.1080/15440478.2017.1414658

Published online: 20 Dec 2017.

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JOURNAL OF NATURAL FIBERS
https://doi.org/10.1080/15440478.2017.1414658

Effect of Green Gram Husk Nanocellulose on Banana Fiber

Composite
Mounika Movvaa and Ravindra Komminenib
a
Mechanical Department, PVP Siddhartha Institute of Technology, Vijayawada, Andhra Pradesh, India; bMechanical
Department, RVR & JC College of Engineering, Guntur, Andhra Pradesh, India

ABSTRACT KEYWORDS
Nanocellulose is a significant bio entity in the present-day applications of Nano; cellulose; green gram
nanocomposites. In this regard, the present work focuses on fabrication of husk; banana composite;
green gram husk cellulose-based hybrid nanocomposites. In the process of tensile strength; hybrid
nanocellulose extraction, residues obtained after each stage of treatment 关键词
are characterized through physical and morphological tests. Later, nanocel- 纳米技术; 纤维素; 绿豆皮;
lulose is reinforced in unsaturated polyester with 1, 3, 5, and 7 wt. % to 香蕉复合; 抗拉强度; 混合
study the tensile properties. The peak tensile strength is found to be 39 的
MPa at 5wt% of cellulose nanocomposites. Noting the enhancement in
tensile properties of nanocomposites, nanocellulose is reinforced in banana
fiber composites and its influence on mechanical properties is studied.
Nanocellulose/banana fiber hybrid composites showed enhanced tensile
strength, flexural strength, and impact strength.

关键词
纳米纤维素是当今纳米复合材料中一个重要的生物材料。在这方面，目
前的工作重点是制备绿豆壳纤维素基杂化纳米复合材料。在纳米纤维素
提取过程中，通过物理和形态测试，对各处理后得到的残渣进行了表
征。随后，在1, 3, 5和7重量%的不饱和聚酯中增强纳米纤维素以研究其拉
伸性能。峰值强度是在5wt%纤维素纳米复合材料39mpa。注意到纳米复
合材料拉伸性能的增强，纳米纤维增强了香蕉纤维复合材料，并研究了
其对力学性能的影响。纳米纤维素/香蕉纤维混杂复合材料的拉伸强度、
弯曲强度和冲击强度均有所提高。

Introduction
World cultivation offers great source of agricultural wastes. Tons of agro wastes are produced every
year, while being processed to products/food. Effective utilization of agricultural wastes which are
available in the form of bagasse, husk, stem etc. would be more beneficial and economical. A series of
scientists emphasized research on chemistry, biochemistry, and material science of agricultural
wastes, especially on cellulose from wastes (Paakko et al. 2007). Cellulose is a structural component
in every plant and it offers unique advantages such as availability, renewability, and environmental
friendliness. Hence, it serves as a low-cost reinforcement for composite materials.
Cellulose nanofibers are reinforced in unsaturated polyester resin and its dynamic mechanical and
thermo-mechanical properties are evaluated by Lavoratti, Scienza, and Zattera (2016). Khan et al.
work reflected increase in tensile strength at 5% (w/w) of nanocellulose chitosan composites (Khan
et al. 2012). On the other hand, details of preparation of micro-crystalline cellulose and nanocellu-
lose from fibrous materials and their subsequent application in composite and allied applications

CONTACT Mounika Movva movva.mounika@gmail.com Mechanical Department, PVP Siddhartha Institute of Technology,
Vijayawada, Andhra Pradesh,India
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/wjnf.
© 2017 Taylor & Francis Group, LLC
2 M. MOVVA AND R. KOMMINENI

have been summarized in a recent publication (Samanta, Basak, and Chattopadhyay 2015).
Cellulose-based nanocomposites are applied in electronics, catalysis, biomedical, tissue engineering
scaffolds, and energy applications.
Green gram husk of 150–200 g can be obtained from 1 kg of whole green grams (Bora et al. 2010).
Cellulose, lignin, and hemicellulose are the key components of green gram husk of which cellulose
constitutes to 45% (Chopra 2012). Besides, cellulose could be hybridized with natural fibers to
improve the properties of composites. Low cost and low density allow natural fiber-based composites
to be used by automotive companies. In specific, banana-polymer composite is one such low cost,
low density and abundantly available natural fiber-based composite which is used as car mat by Ford
Lincoln (Assis et al. 2015).
The properties of any composite depend not only on reinforcement, but also on matrix material.
Unsaturated polyester resin offers good mechanical properties and dielectric strength when com-
bined with cellulose and natural fibers like bamboo, sisal, sanseviera, vakka, etc. Unsaturated
polyester resin is cost effective and exhibits room temperature curing ability with best properties
(Mounika and Ravindra 2015, 2017).
Surveying the extent of research covered in the field of cellulose nanocomposites, the present
work aims to determine the mechanical properties of banana fiber-based polyester composite by
adding nanocellulose as filler. Nanocellulose is extracted from green gram husk through chemical
treatment and is characterized by physical and morphological tests at various stages of chemical
treatments. In addition, cellulose nanocomposites and banana fiber/cellulose nanocomposites,
mechanical behavior was studied through various tests.

Experimental
Casting materials and chemicals
Unsaturated polyester resin (Pumax, India) with specific gravity of 1.13 and viscosity of 380mPas
under atmospheric conditions and the reagents 97% NaOH, 98% H2SO4, and 30% w/v H2O2 are
procured from Chem Tech, India.

Plant materials
Green gram husk is used to extract nanocellulose. While, the husk is obtained either from gram
milling companies or by soaking the whole seeds that are purchased from local market in water.
Soaking the whole seeds overnight, separating the husk through manual efforts and drying the husk
in sun to remove the moisture in it, all these steps make the husk ready for extraction.

Isolation of nanocellulose and fabrication of nanocomposite

Acid catalyzed hydrolysis is used to extract nanocellulose as described in literature (Elanthikkal et al.
2010). Husk is initially treated with 10 wt.% NaOH for 3 hr at 70°C. Alkali treatment removed
hemicellulose to a greater extent, and after alkalization the residue is treated for half day with 50 ml
of 30 wt% H2O2 at 70°C. Bleaching process whitens the residue, removes lignin, and also dissolves
left over hemicellulose. The centrifuged residue that is cellulose is stirred with 50 ml of 64 wt%
H2SO4 solution at 70°C for 30 min through which amorphous regions of cellulose are deprived.
Lastly, the residue is washed with water until the pH becomes neutral and is ball milled to nanosize.
To destroy the aggregates and disperse the suspension uniformly, the nanocellulose is mixed with resin
thoroughly using probe sonicator. Later, nanocellulose-resin mixture is stirred with the 1.5% of accelerator
and catalyst, respectively. Accelerator and catalyst are added just before pouring the resin mixture into the
moulds to cure the samples. A get coat is applied to the sides of moulds, so that the sample could be easily
taken out after curing. Moulds of 162 × 90 x 3 mm dimensions are prepared for tensile samples. The resin
 JOURNAL OF NATURAL FIBERS 3

mixed with 1% nanocellulose is poured into moulds and is allowed to cure at room temperature for
20–24 hr. The cured composite was cut to specimens based on ASTM standards and are tested 3 days after
curing. Similarly 3, 5, and 7wt% of cellulose-reinforced polymer nanocomposites are prepared using hand
lay-up technique (Masoodi et al. 2012). In case of Banana fiber/Nanocellulose based composite, hand lay-up
method is used to fill up the mould with appropriate amount of nanocellulose-resin mixture and banana
fibers, while the samples start and end with the layers of resin mixture. Banana fibers are aligned parallel to
each other with 0° orientations that are along the axial direction of the mould.

Characterization
Scanning electron microscopy (SEM) analysis
High-resolution surface imaging is used for SEM analysis. SEM analysis of nanocellulose is done on
the equipment that has magnification of range 5x to 300,000x both in high and low vacuum modes.
JEOL Model, JSM-6390LV, USA has compatibility to work at 3 nm about resolution. The samples
are coated with thin gold film and the images are taken at an accelerating potential of 20 kV.

X-ray diffraction (XRD)

Crystallinity index of nanocellulose is resolved by using X-ray diffractometry technique. Bruker AXS,
D8 Advance, USA is equipped with CuKα emission. Scattered radiation is sensed in the range
2θ = 3–80° at a working voltage of 35 kV and current is 35 mA. The step size for noting the degree of
crystallinity is 0.02° under a scanning rate of 1°/min.

Fourier transform infrared spectroscopy (FTIR)

KBr beam splitter Thermo Nicolet, Avatar 370, USA is utilized for defining functional groups. The
model shows a spectral range of 4000–400 cm−1 with a resolution of 4 cm−1. At every stage of
treatment, 32 scans are taken for each sample and to equip convenient measurement, DTGS
Detector and HATR Assembly are added.

Thermogravimetric analysis (TGA)

TGA is performed to study thermal degradation behavior. Perkin Elmer, Diamond TG/DTA model,
USA is used to study degradation behavior by heating the sample from 40°C to 730°C at 20°C/min
under nitrogen atmosphere with a gas flow of 20 ml/min.

Tensile test
Samples of 160mm x 12.5mm x 3mm dimensioning are cut from composite slab. The samples are
glued with aluminium strips in order to provide perfect gripping. 20KN-Electronic tensometer,
Kudale Instruments, METM 2000 ER-1 model, India which is working at a crosshead speed of 2mm/
min is used to test the tensile strength and flexural strength of biocomposites while changing the
attachments. Instead of feasibility of machine, samples are prepared as per ASTM D-638 standards
and a cell load of 10N is applied progressively while testing.

Flexural test
Three-point bend test and four-point bend test are two kinds of bend tests, of which, three-point
bend test is often considered, to determine the flexural strength of biocomposites. However, there is
a cause behind the choice of three point bend test that is, low material requirements and easiness in
4 M. MOVVA AND R. KOMMINENI

testing. Load is applied at the mid-section of samples in perpendicular direction. As per ASTM D790
standards, the samples should have the dimensions of 100mm x 25mm x 3mm.

Impact test
According to ASTM D 256M standards, samples of 63.5mm long, 12.7mm deep, and 10mm wide
are fabricated and V-notch of 45° is made with a file at the 90° saw cut to the sample axis. The
purpose of v-notch is to initiate the crack. Izod impact strength is tested on International
Equipments, Impact Tester, India.

Results and discussion

Morphological analysis
Fig.1a shows the SEM image of green gram husk, which clearly reveals that the cellulose and non-
cellulosic constituents are cemented together. Non-cellulosic constituents such as lignin, hemicellu-
lose, and other extractives are removed through various steps of chemical treatment (Xiao et al.
2016). Firstly, raw green gram husk is treated with NaOH to dissolve hemicellulose and other
extractives. Figure 1b serves as an evidence for hemicellulose removal, as the figure visibly pictures
the disintegrated matter. The next step of chemical treatment is bleaching, during which lignin and
remaining hemicellulose are removed to all possible extent (Chirayil et al. 2014). As a result,
Figure 1c exhibits the cellulose that is eventually delinked from the non-cellulosic constituents.
Finally, acid hydrolysis deprives the amorphous regions of cellulose as crystalline regions of cellulose
remains undissolved up to a definite acid concentration, time of hydrolysis, and temperature.
Therefore, crystalline regions of the cellulose are perked up and Figure 1d shows the acid hydrolyzed
and milled nanocellulose (NC). ImageJ software is used to obtain a histogram that shows size
distribution of nanocellulose (Neto et al. 2013). Therefore, from Figure 1e it is observed that
cellulose dimensions fall in nano-range.

XRD studies
XRD patterns at different stages of chemical treatment are shown in Figure 2. The key peak observed
at 2θ = 22° and a shoulder in the region 14–17° signify the existence of cellulose I. Crystallinity index
(CrI) is attained by substituting the 200 peak value and dip value between the 200 and 110 peaks in
the following equation.
I200  Iam
CrI ¼  100
I200
where, I200 represents crystalline and amorphous regions; Iam represents amorphous regions.
Crystallinity index is useful only for assessment purpose as it presents semi-quantitative assess-
ment of cellulose. When compared to alkali treated and bleached samples, acid hydrolyzed sample
showed increased crystallinity index. Increase in crystallinity index is due to the removal of non-
cellulosic constituents and amorphous regions of cellulose (Mondragon et al. 2014). Crystallinity
index shown by untreated, alkali treated, bleached, and acid hydrolyzed cellulose are 59, 64, 67, and
73%, respectively. Crystallinity index of 73% is for 30 min acid hydrolysed cellulose. However,
crystallinity indices shown by corncob at different hydrolysis times that is, when cellulose is
hydrolysed for 30, 60, and 90 min, are dissimilar. Maximum crystallinity index is seen for 60 min
treatment and for 90 min long the index value turned down as both amorphous and crystalline
regions are destroyed. Hence, crystallinity of green gram husk can be further improved by treating it
for optimum excess time (Silverio et al. 2013).
 JOURNAL OF NATURAL FIBERS 5

a b

20-30 30-40 40-50 50-60 60-70 70-80

Width (nm)

Figure 1. SEM images for a) raw, b) alkali treated, c) bleached, and d) acid hydrolyzed cellulose e) width of nanocellulose
calculated using ImageJ.

FTIR spectroscopy analysis

Figure 3 shows FTIR spectra obtained for untreated, alkali treated, bleached, and acid hydrolyzed
matter of green gram husk. The spectra at 1060 cm−1 corresponds to O-H stretching in cellulose. The
band initiated at 1179 cm−1 is due to the stretching of aromatic ring of lignin. Yet, subsequent to
bleaching the peak at 1179 cm−1 was vanished and this marked the elimination of lignin. The crest at
3481 cm−1 is coupled with O-H stretch in cellulose. Bending vibration of absorbed water molecules
and C = O bonds of hemicellulose are observed at 1640 cm−1 peak (Mandal and Chakrabarty 2011).
A small shoulder positioned at 1745 cm−1 representing hemicellulose is departed after alkali treat-
ment. Basically, 1768 cm−1 is allied with carbonyl groups of hemicellulose and p-coumaric and
ferulic acids of ester linkage carboxylic groups. However, carbonyl group is important element of
hemicellulose, and carboxylic group is significant component for hemicellulose and/or lignin. As
6 M. MOVVA AND R. KOMMINENI

Lin (Counts)
d
c
b
a

3 23 43 63
2 Theta - Scale
Figure 2. XRD for a) raw matter, b) alkali treated, c) bleached, and d) acid hydrolyzed cellulose.

d
Transmittance (a.u)

4000 3000 2000 1000 0

Wavelength (cm-1)
Figure 3. FTIR images for a) raw matter, b) alkali treated, c) bleached, and d) acid hydrolyzed cellulose.

alkali treatment removed the peak at 1768 cm−1, this removal can be regarded as removal of
dominant constituent that is hemicellulose (Mondragon et al. 2014). The band at 2900 cm−1
represents C-H in cellulose, hemicellulose, and lignin. Lastly, bleached and acid hydrolyzed cellulose
showed almost same FTIR spectra in the peaks.

Thermogravimetric analysis (TGA)

Figure 4 shows the thermal degradation curves after each and every stage of chemical treatment.
Every thermal degradation thermograph showed two stages of weight loss. The first stage of
weight loss is witnessed within a temperature range of 60–180°C which is 11, 8, 5, 4.5% for
untreated, alkali treated, bleached, and acid hydrolyzed cellulose, correspondingly. This stage of
weight loss in any matter is strongly due to the evaporation of water. From the weight loss
percent numerical, it is clear that cellulose retains lower moisture content as bringing in sulfate
 JOURNAL OF NATURAL FIBERS 7

Figure 4. TGA images for a) raw matter, b) alkali treated, c) bleached, and d) acid hydrolyzed cellulose.

ester groups during acid hydrolysis and removal of non-cellulosic constituents have dehydrated
the nanocellulose (Zuluaga et al. 2009). In the second stage of weight loss, raw husk deprivation
started so earlier when compared to treated residues as non-cellulosic constituents exhibit lower
thermal stability than cellulose. After further steps of treatment, the degradation temperature of
cellulose amplified noticeably, as non-cellulosic elements are being separated and crystallinity is
being increased (Oun and Rhim 2016).
The zenith degradation temperatures could be obtained by considering derivative weight
percent versus temperature intrigue. 301, 333, 354, and 361°C are the peak degradation tem-
peratures shown by raw, alkali treated, bleached, and acid hydrolyzed cellulose, respectively. In
case of raw matter, hemicellulose is integrated into the structure of the cellulose and provides
more active sites for the thermal degradation to begin. Hence, acid hydrolyzed cellulose shows
highest degradation temperature (Chirayail et al. 2014) and lowest carbon residue, due to the
absence of non-cellulosic components and amorphous regions of cellulose (Nguyen, Zavarin, and
Barrall 1981).

Mechanical properties of nanocomposites

Nanocomposites with 1, 3, 5, and 7% (w/w) of nanocellulose are fabricated to determine its tensile
strength, tensile modulus, and elongation at break. Tensile strength of nanocomposites increased up
to 5% of nanocellulose and decreased with further increase in nanocellulose percent, as shown in
Fig. 5. The tensile strength of pure unsaturated polyester resin is found to be 20 MPa. The highest
tensile strength noted at 5% of nanocellulose is 39MPa. When compared to matrix material, the
tensile strength at 5% nanocellulose is 95% higher (Figure 5a). Crowning TS is attained due to
superior crystallinity index of cellulose and strong bonding between reinforcement and matrix (Hajji
et al. 1996). The key causes for improvement in tensile strength are due to uniform dispersion of
cellulose and transfer of stress applied on resin to structurally strong nanocellulose. Nevertheless, the
TS decreased at maximum weight fraction of nanocellulose, due to insufficient adhesion and
aggregation of nanocellulose, as aggregation increases the local stress concentration areas (Haafiz
et al. 2013)
Tensile modulus also showed similar trend as tensile strength. Tensile modulus value of unsatu-
rated polyester is 236MPa. The incorporation of 5% of nanocellulose caused a significant increase in
8 M. MOVVA AND R. KOMMINENI

45

Tensile Strength (MPa)

40

35

30

25

20
0 1 2 3 4 5 6 7 8
Weight Percent of nanocellulose
Figure 5a. Variation of tensile strength with weight percent of nanocellulose.

Tensile Modulus
1200 12

Elongation at break (%)

Tensile Modulus (MPa)

1000 10
800 8
600 6
400 4
200 2
0 0
0 1 2 3 4 5 6 7 8
Weight Percent of nanocellulose
Figure 5b Variation of tensile modulus and elongation at break with wt.% of nanocellulose.

tensile modulus, which is 1083MPa (Figure 5b). Frequently, addition of nanocellulose increases
brittleness of biocomposite. However, tensile modulus of biocomposites shows increasing trend
when low nanocellulose content is added. This effect may be attributed to the increased stiffness
of composites (Khan et al. 2012) Therefore, with further addition (>5%) of nanocellulose, tensile
modulus values are thoroughly declined due to stress concentration areas (Huq et al. 2012)
 JOURNAL OF NATURAL FIBERS 9

Elongation at break decreased with increase in nanocellulose in unsaturated polyester matrix.

This effect could be attributed to strong interaction between the reinforcement and matrix,
which restricts the mobility of polymer chains under loading.

Effect of cellulose on the morphology of the fracture surface of nanocomposites

The SEM micrographs of fractured surface of cellulose-based nanocomposites are shown in Figure 6.
The surface of 1, 3, and 5% nanocomposites is smooth as shown in Figure6a–c. Figure 6a–c,
intensely represent the improved interaction between reinforcement and matrix material. Also, the
mechanical properties of nanocomposites are amplified with increased uniform dispersion of
nanocellulose in matrix material. However, Figure 6d shows the rough surface with ripples and
ridges at cellulose concentrated sites, because of which density of crack deflection sites are increased.
This effect is due to high cellulose loading and aggregation of nanocellulose, for which cellulose and
polymer compatibility is lowered. Subsequently, the mechanical properties showed declining trend at
7% of cellulose (Khan et al. 2012).
It is clearly evident from Figure 6b and 6c that the nanocellulose is well dispersed and plastered by
matrix. Therefore, perfect plastering and dispersion improves the adhesion between reinforcement and
matrix and no pull out of nanoparticles or debonding is observed. On the other hand, excess additions of
nanocellulose results in debonding and pull out of matter as seen in Figure 6d. These images demon-
strated a similarity with the tensile results of the nanocomposites (Kaushik, Singh, and Verma 2010).

a b

c d

Figure 6 SEM micrographs of fractured surfaces of a) 1% NCb) 3% NC c) 5% NC and d) 7% NC.

10 M. MOVVA AND R. KOMMINENI

Mechanical properties of hybrid nanocomposites

Tensile test
Addition of nanocellulose improved the tensile properties of matrix material. Considering the effect
of nanocellulose addition, nanocellulose is added to banana fiber composites. Tensile strength of
nanocellulose/banana fiber composites with respect to varying weight percent of nanocellulose is
shown in Figure 7a. While, banana fiber weight percent is kept constant, that is 10% with respect to
matrix. This combination of composites showed considerable enhancement in properties, but
peculiarly the improvement is observed at 10% of banana fiber and 3% of nanocellulose and this
value of tensile strength is 69% higher than cellulose nanocomposites. The high tensile strength
encountered at 3% of nanocellulose is due to the strong interface bonding between reinforcement

65
60
Tensile Strength (MPa)

55
50
45
40
35
30
0 1 2 3 4 5 6 7 8
Weight Percent of nanocellulose
Figure 7a Variation of tensile strength with respect to weight percent of filler.

1400

1200
Tensile Modulus (MPa)

1000

800

600

400

200
0 2 4 6 8
Weight percent of nanocellulose
Figure 7b Variation of tensile modulus with respect to weight percent of filler.
 JOURNAL OF NATURAL FIBERS 11

and resin. In turn, weak interfacial bonding between hydrophobic resin and hydrophilic fiber is also
reduced by the addition of crystalline nanocellulose. However, again excessive aggregation of
cellulose and banana fibers prevented proper wetting of reinforcement with resin and showed
decrease in tensile strength (Pawel and Flodin 1986). On the other hand, tensile modulus of
nanocellulose-based composite shown in Figure 7b exhibited similarly tendency.

Flexural test
Flexural strength shown in Figure 8 of cellulose nanocomposites and banana fiber/cellulose nano-
composites shows the same drift as that of tensile strength and tensile modulus of cellulose
nanocomposites and banana fiber/cellulose nanocomposites respectively. Straining the mid-span of
the samples, by applying flexural loads shows the deflection at every point loading. Cellulose of
nanosize and high crystallinity index shows significant effect on the flexural behavior of composites.
Highest flexural strength of banana fiber/nanocellulose composite is 109MPa at 3% of cellulose
which is 51% higher than nanocellulose composite (Noorunnisa et al. 2007).

120
Flexural Strength (MPa)

110
100
90
80
70
60
50
40
30
0 2 4 6 8
Weight percent of nanocellulose
Figure 8 Variation of flexural strength with respect to weight percent of filler.

70
Impact strength (J/m)

60
50
40
30
20
10
0
Banana fiber Banana fiber NC Comp
+ NC Comp Comp
Figure 9 Comparison of impact strengths of different composites.
12 M. MOVVA AND R. KOMMINENI

Impact test
Impact of banana fiber, banana fiber/NC and NC if reinforced in polyester resin is observed in
Figure 9. And their impact on impact strength is considerable, the hybridization of materials resulted
in significant enhancement (Mohammad et al. 2011). Banana fiber/nanocellulose composite, banana
fiber composite, cellulose composite, over these series of materials hybridization or addition of filler
to banana fiber composite showed vast effect on the impact strength that is 57 J/m is noted.

Conclusion
Material characterizing tests such as SEM, FTIR, XRD, and TGA reveals that nanocellulose is
successfully extracted from green gram husk through various chemical treatments. In turn, extracted
nanocellulose exhibited higher crystallinity and thermal stability. Hence, reinforcement of crystalline
nanocellulose in polymer matrix improved the tensile strength and tensile modulus of nanocompo-
sites upto 5% of nanocellulose. The effect of nanocellulose on mechanical behavior is also better
understood with fracture surface SEM micrographs. Nanocellulose/banana fiber hybrid composites
also showed significant enhancement in tensile, flexural, and impact strengths. Therefore, these
cellulose-based nanocomposites and hybrid nanocomposites with noteworthy properties can find its
application in the field of engineering and these composites being agrowaste based they could add
commercial value to the crop.

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