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Abstract: A natural long staple ligno-cellulosic fibers have been extracted from the cornhusks using an alkali treatment.
Physico-chemical properties such as chemical composition, length, fineness, crystallinity, surface properties, etc. measured by
standard methods are reported in this paper. The physico-chemical and morphological properties of the extracted cornhusk
fibers are discussed in detail and compared with other cellulosic like cotton and ligno-cellulosic fibers such as jute. Scanning
electron microscopy was used to study the morphological and cross-sectional view and energy dispersive X-ray and FTIR
were used for the identification and quantification of elements, groups present in the cornhusk and other cellulosic and ligno-
cellulosic fibers. In addition, fibers are characterized by thermo-gravimetric analysis. Results showed that morphological and
physico-chemical behavior is more or less similar to other multicellular ligno-cellulosic fibers like jute.
Keywords: Cornhusk fibers, Physico-chemical properties, Ligno-cellulosic fibers, XRD, SEM
687
688 Fibers and Polymers 2016, Vol.17, No.5 Nishant Kambli et al.
Microscope (FEG-SEM) to determine the quantity of the 100 oC is insufficient for extraction of fibers from cornhusk,
elements present on the fiber surface and expressed in whereas the cornhusk fibers extracted from 100 g cornhusks
atomic and weight percent. at 120, 140, and 160 oC are 32.01, 23.02, and 22.953 g
respectively. However, cornhusk fibers extracted at higher
Morphological Structure temperatures (140 and 160 oC) is brownish in nature and
The morphological structure of the fibers and its cross very harsh and brittle as depicted in Figure 1(B) and (C). It
section were studied using a scanning electron microscope may be due to the removal of lignin present in the cornhusk
(SEM), Philips XL-30, with an accelerating voltage of fiber. Therefore, further technical experiments were carried
12 kV. Each sample was coated with a thin layer of conducting out with the yellowish cornhusk fibers extracted at 120 oC,
material (gold/palladium) using a sputter coater before SEM as shown in Figure 1(A). Some part of extracted fibers were
measurement. further bleached with 6 % hydrogen peroxide (H2O2) to
impart whiteness to the fibers. The bleaching process was
TG Analysis in N2 Atmosphere carried out for 60 min at 85 oC using 1 g/l concentrations of
Thermogravimetry measures the gradual weight loss of a sodium hydroxide (NaOH) with the material:liquor ratio of
sample with respect to time at a constant heating rate. The 1:20. NaOH is used to bring the pH up to 9-10 because H2O2
TG curves of the cornhusk fibers were obtained using a becomes active at this pH. High pH and temperature lead to
thermogravimetric analyzer (METTLER TOLEDO TG-50/ the faster decomposition of peroxide bleaching liquor and
MT5) in a nitrogen atmosphere with 2 ml/min flow rate and degradation of cellulose. To overcome this problem sodium
a constant heating rate of 10 oC/min. silicate (1.5 g/l) is used as a stabilizer to control or regulate
these effects.
AFM Analysis of Cornhusk Fiber Cornhusk fiber extraction parameters such as % weight
The AFM analysis of cornhusk fiber was carried out using loss and % fibers recovered are given in Table 1. It was
an Innova AFM (Veeco, Santa Barbara, CA, US) equipped found from the table that at 10 % NaOH with 120 oC is an
with a 90 μm scanner. A cornhusk fiber was placed onto a ideal condition for the extraction of the cornhusk fibers.
freshly cleaved mica surface and air dried. All images were
obtained using a tapping mode at room temperature. The Properties and Fiber Composition
silicon nitride cantilever with a spring constant of 40 Nm-1 Fiber composition affects appearance, structure, properties,
was used. The scan rate of 1.0 Hz and 512 lines per 5 μm and processability of the fiber. The composition and properties
was used for optimum contrast. No filtering was used during of the extracted cornhusk fibers are evaluated and compared
scanning. with cellulosic cotton and ligno-cellulosic jute fiber (Table
2). The parameters of cotton and jute fibers reported here in
Results and Discussion Table 2 for comparison purpose are taken from the literatures
[9,10]. The cornhusk fiber contains 50-55 % cellulose,
Fiber Extraction whereas cotton and jute fibers contain around 85-90 and 51-
Different experiments were carried out to standardize the 72 % cellulose, respectively. Lignin, the binding substituents
suitable conditions for extraction of fibers from cornhusks. which hold the individual cells together, is present in jute
The experiments were carried out for 60 min at four different and cornhusk fibers. As far as the crystallinity is concerned,
temperature levels viz. 100, 120, 140, and 160 oC using 10 % cornhusk fiber is less crystalline (56.9 %) than the cellulosic
w/w concentrations of sodium hydroxide (as an alkali cotton fiber, which might be due to the presence of more
material for degumming and releasing the fibers from amorphous hemi-cellulose and lignin in it. The crystallinity
cornhusks) 5 g/l with the material:liquor ratio of 1:20. As far of cornhusk fiber is comparable with that of jute fiber.
as the extraction temperature is concerned, it was found that Crystallinity of cornhusk fiber has been confirmed by X-ray
Figure 1. Cornhusk fibers extracted from cornhusks at (A) 120 oC, (B) 140 oC, and (C) 160 oC and (D) extracted at 120 oC and bleached.
690 Fibers and Polymers 2016, Vol.17, No.5 Nishant Kambli et al.
Table 1. Extraction of the cornhusk fiber at different temperatures and alkali concentrations
NaOH (%) on Temperature % wt. loss of
Sr. no. % fibers recovered Remarks
wt. of fibers (oC) cornhusk
1 7 120 - - Non extractable
2 8 120 - - Non extractable
3 9 120 65.0 35.0 Extractable
4 10 120 68.0 32.0 Extractable (good quality)
5 7 140 - - Non extractable
6 8 140 69.1 30.9 Extractable
7 9 140 69.9 30.1 Extractable
8 10 140 77.0 23.0 Extractable
9 7 160 66.5 33.5 Extractable
10 8 160 70.8 29.2 Extractable
11 9 160 70.9 29.1 Extractable
12 10 160 77.0 23.0 Extractable
Note: M:L=1:20, wetting agent=1 g/lit, incubation period=1 hr.
Table 2. Fiber composition and properties of cornhusk fiber and its comparison with other fibers
Sr. no. Parameters Cornhusk Jute Cotton
1 Length (mm) 40-180 150-360 10-35
2 Diameter (µm) 130-140 (33.0) 15-25 11-22
3 Lignin (%) 7.5 5-13 0
4 Cellulose content (%) 50-55 51-72 85-90
5 Hemicellulose content (%) 39.39 12-20.4 4-6
6 Holocellulose content (%) 89.72 - -
7 Crystallinity (%) 56.9 50-55 65-70
8 Tenacity (g/den) 1.3 (30.6) 4-5 3-5
9 Elongation (%) 19.7 (31.1) 0.9-1.2 5-10
10 Modulus of rigidity (g/den) 128.9 (24.7) 180-200 50-60
11 Work of rupture (g·cm/den) 0.39 (26.3) 0.03 0.11
12 Linear mass density (tex) 29.7 1.25-5 0.1-0.3
13 Absorbency (sec) 0.92 Absorbent Absorbent
14 Ash content (%) 1.16 0.9-1.1 1.1-1.8
15 Moisture content (%) 11.4 12-14 6-8
16 Moisture regain (%) 12.9 13.8 7.0-8.5
Note: Figures in the parenthesis indicate C.V. (%).
diffraction represented in Figure 2. Because of less presence of encrusting substances that give cornhusk a
crystallinity as compared to cotton fibers, cornhusk fiber is rough and irregular appearance. On the contrary, grey ligno-
more accessible to water, dyes, and other finishing chemicals. cellulosic jute and banana fibers showed comparatively
In regards to fineness cornhusk fiber is coarser than cotton smooth, regular surface appearance. Cotton fibers showed
and jute fibers. The diameter of the cornhusk fiber is also even cleaner and smoother surfaces. Non-cellulosic material
larger than cotton and jute fibers. present at the fiber surfaces may be responsible for this kind
of morphological observations. Those encrusting non-
SEM Analysis cellulosic substances may be carbon based, which has been
SEM images of the chemically extracted cornhusk fiber further confirmed by EDX analysis in the later part of this
showed rough, distorted, honeycomb nest like cellular paper. As far as the morphology of the cross-sectional view
structure with the presence of small micropits on the fiber of the cornhusk fiber (Figure 4(A1)) is concerned, it showed
surface as depicted in Figure 3(A). It may be due to the central hollow regions like banana fiber. This hollow regions
Extraction of Fibers from Cornhusk and Its Properties Fibers and Polymers 2016, Vol.17, No.5 691
FTIR Analysis
FTIR spectra of cornhusk, jute, and cotton fibers were
recorded to understand the chemical groups present in each
fiber (Figure 5). FTIR spectra of cornhusk and cotton fibers
(Figure 5(A) and (C)) show a broad absorption band around
3200-3498 cm-1 corresponding to the OH stretching of
hydroxyl group of cellulose. However, jute contains less
amount of hydroxyl groups as seen in Figure 5(B). Peak
Figure 2. X-ray diffraction pattern of the extracted cornhusk corresponding to the CH stretching at 2875 cm-1 is more
fibers. intense in cotton and cornhusk fibers, which may be due to
Figure 3. SEM images of (A) cornhusk, (B) jute, (C) cotton, (D) banana, and (E) coir fiber.
Figure 4. Surface morphology of the cross-section of (A1) cornhusk, (B1) jute, (C1) cotton, (D1) banana, and (E1) coir fiber.
692 Fibers and Polymers 2016, Vol.17, No.5 Nishant Kambli et al.
the presence of more cellulosic -CH2OH groups, whereas the EDX Analysis
broad peak at 1650 cm-1 is attributed to the C=O stretching EDX analysis of chemically extracted cornhusk fibers,
of the carbonyl group present in it and the 1425 cm-1 peak is ligno-cellulosic jute and cellulosic cotton fibers is given in
assigned to CH2 symmetric bending. However, the peak at Table 3. It showed that chemically extracted cornhusk fibers
1425 cm-1 is more prominent in case of cotton fiber, which contain almost 62 % weight of carbon, which is more than
may be because of more cellulose content. The absorption the jute fiber and cotton fiber. It may be due to the presence
peak at 1637 cm-1 is due to the anti-symmetric deformation of more non-cellulosic materials in the cornhusk fiber. On
of C-O-C band in cellulose and hemi-cellulose. It is more the other hand amount of oxygen present is around 36 %,
prominent in cornhusk and cotton fibers, but less prominent which is less than the jute and the cotton fiber. However
in jute fiber. Since the two peaks (1650 and 1637 cm-1) are after bleaching both carbon and oxygen weight percentage
very close, we get a sharp and broad peak due to combined (%) was reduced by 7.8 % and 9.1 % respectively. It might
effect of C=O groups and C-O-C groups. The broad peak be due to the removal of lignin and other non-cellulosic
around 1050 cm-1 is due to C-O and O-H stretching found in materials during bleaching. Further extracted cornhusk fiber
all the fibers, whereas the shoulder peak at 1000 cm-1 found also contain magnesium, silicon, calcium elements, which is
in case of cornhusk fiber is interpreted as C-O-C stretching not present in jute and the cotton fibers. These elements
at the β (1-4) glycoside linkage of cellulose. come from the non-cellulosic cell wall material of the
cornhusk fibers.
Table 3. Atomic and weight percentage of cornhusk, jute and cotton fibers using EDX
Cornhusk fiber (A) Jute fiber (B) Cotton fiber (C)
Elements
Weight (%) Atomic (%) Weight (%) Atomic (%) Weight (%) Atomic (%)
C 62.54 69.17 55.68 62.72 46.1 53.2
O 36.80 30.56 43.89 37.11 53.9 46.8
Na 0 0 0 0 0 0
Mg 0.13 0.07 0 0 0 0
Al 0 0 0 0 0 0
Si 0.20 0.10 0.11 0.06 0 0
P 0 0 0 0 0 0
Cl 0 0 0 0 0 0
K 0 0 0 0 0 0
Ca 0.33 0.11 0 0 0 0
S 0 0 0.18 0.08 0 0
Extraction of Fibers from Cornhusk and Its Properties Fibers and Polymers 2016, Vol.17, No.5 693
TGA Analysis
TGA curves of cotton, jute, extracted cornhusk, and
bleached cornhusk fibers are represented in Figure 7. It was
observed from the Figure 7 that the TG curve of the cotton
fiber (C) showed sharp fall at 370 oC and less amount of char
mass remained at higher temperature, whereas jute and
cornhusk fibers showed fall at 350 oC ((B) and (A)), but here
the rate of fall, i.e., the weight loss rate is lower compared to
the only cellulosic cotton fiber. This particular temperature is
reported as pyrolysis or decomposition temperature of the
cellulose. It means that lignin and non-cellulosic matter
present in jute and cornhusk fibers are responsible for
lowering down the pyrolysis, i.e., (decomposition) temperature
compared to the cotton fiber by 20 oC. Another interesting
observation from the Figure 7 is that the amount of char
mass remained at higher temperature is slightly lower in
case of jute fiber than cornhusk fiber, this might be due to
less amount of lignin present in the jute fiber.
Figure 6. AFM images of (A) cornhusk and (B) jute fibers.
Conclusion
Cornhusk fibers are the only fibers obtained from the by-
product of a food crop with large availability and low cost. It
has low crystallinity and rough surface with hollow cross-
sectional view like ligno-cellulosic banana fibers, which
makes it suitable for more chemical and dye absorption.
SEM topography of the cornhusk fiber showed rough,
encrusting surface due to the presence of non-cellulosic
materials. As far as the thermal stability and chemical
composition is concerned, it showed almost similar properties
like jute. As far as the strength of the cornhusk fiber is
concerned, it showed less tensile strength and more elongation
than jute and cotton fibers.
Acknowledgement
5. N. Reddy and Y. Yang, Trends Biotechnol., 23, 22 (2005). 10. G. A. Serad and J. R. Sanders in “Encyclopaedia of
6. N. Reddy and Y. Yang, AATCC Review, 5, 24 (2005). Textiles, Fibers and Nonwoven Fabrics” (M. Grayson Ed.),
7. N. Reddy and Y. Yang, Indian J. Fibre Text. Res., 31, 537 pp.62-89, Wiley-Interscience Publication, New York, 1984.
(2006). 11. E. Canetta, K. Montiel, and A. K. Adya, Forensic Sci. Int.,
8. G. Halliwell in “Methods of Enzymatic Analysis”, (H. U. 191, 6 (2009).
Bergmeyer Ed.), pp.66-67, Academic Press, New York, 12. S. O. Han and H. Y. Choi in “Microscopy: Science,
1965. Technology, Applications and Education” (A. Mendez-
9. J. Biagiotti, D. Puglia, and J. M. Kenny, J. Nat. Fibers, 1, Vilas and J. Diaz Eds.), pp.1880-1887, Formatex Research
37 (2004). Center, 2010.