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Synthesis and Characterization of Coconut Shell Ash

Article  in  Journal of Nanoscience and Nanotechnology · July 2019

DOI: 10.1166/jnn.2019.16299

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 Article
Journal of
Copyright © 2019 American Scientific Publishers
Nanoscience and Nanotechnology
All rights reserved Vol. 19, 4123–4128, 2019
Printed in the United States of America www.aspbs.com/jnn

Synthesis and Characterization of Coconut Shell Ash

M. Satheesh1 ∗ , M. Pugazhvadivu1 , B. Prabu1 , V. Gunasegaran2 , and A. Manikandan3
1
Department of Mechanical Engineering, Pondicherry Engineering College, Puducherry 605014, India
2
Department of Mechanical Engineering, BSA Crescent Institute of Science and Technology, Chennai 600048, India
3
Department of Chemistry, Bharath Institute of Higher Education and Research, Chennai 600073, India

Synthesizing Coconut Shell Ash (CSA) is a kind of manufacturing the powder form ash material
which can be incorporated in the composite as reinforcement. This ash material used to improve the
mechanical properties of metals when added in Metal Matrix Composite’s (MMC’s) based prepara-
tion. The fabrication of CSA powder is the preparatory functional part, because it varies its properties
based on the manufacturing method. In this work, a novel method is used to manufacture the ash
powder and to study the physical and chemical properties of CSA particles. CSA particles are syn-
thesized in open fire hearth. Physical properties such as pH, ash content, moisture content, loss on
ignition, density, surface area, pore volume and pore dia were studied. Chemical characterization
study is carried out for chemical composition analysis, the morphology of ash particles, percent-
age of various elements present and various chemical functional groups present in the samples
through XRF, SEM/EDS and FTIR techniques respectively. Crystallite structures, average particle
size, and thermal stability of CSA were investigated by XRD and TGA methods. The result shows
that the total maximum IP:percentage
5.189.201.171 2 , Al2Mon,
of SiOOn: O3 and18Fe 2 O3 2019
Mar (∼84%) will increase the strength of
07:12:08
MMC’s. The total percentage Copyright:
of Ca andAmerican
K is minimumScientific Publishers
than the other CSA preparation methods, so
Delivered
that it will reduce the corrosion. And also producebylowIngenta
density ash powder (1.65 gm/cc) which will
reduce the weight and density of MMC’s. This CSA powder can be used in MMC where maximum
strength–weight ratio and wear resistance is required.
Keywords: Ash Properties, Coconut Shell Ash, Nanomaterials, SEM, XRD, FTIR.

1. INTRODUCTION energy productions. Agro waste ash is one of the main

Coconut shell is an agricultural waste and it can be re- reinforcement material used in Metal Matrix Composites
used in engineering applications. Approximately, 15 Kg of (MMCs), because of its low density, low cost produc-
coconut shell is obtained from 100 Kg of coconut. Culti- tion and easy availability. Few researchers have examined
vation of coconuts has been done in more than 90 coun- coconut shell ash and they found that the SiO2 (45.05%,
tries worldwide on about 10 million hectares. Indonesia, 66.5% and 14%),2 10 11 is a major constituent in coconut
Philippines and India accounts for almost 75% of world’s shell ash. SiO2 varies in different weight percentage based
coconut production.1 2 Coconut shell contains organic and on their cultivation region, basic shell properties and ash
inorganic material and the organic materials in coconut powder manufacturing techniques. Coconut shell mainly
shells are 33.61% Cellulose, 36.51% Lignin, 29.27% Pen- contains carbohydrate materials and these materials are
tose’s and 0.61% ash.3 Many agro waste materials are completely burned to get coconut shell ash particles at
available like rice husk,4 bamboo leaves,5 palm kernel micro level. Synthesized micro level CSA particles can be
and rice straw etc. These agro waste materials are used converted in to nano size CSA particles by using plane-
to make ashes which contains metals in oxide form like tary ball milling process.12 While using micro and nano
SiO2 , Al2 O3 , Fe2 O3 , TiO2 , K2 O, CaO, ZnO, MnO etc. level CSA particles in composite materials, the grain size
The ash is used in various applications like cement based and weight% of the matrix material will decrease due to
materials manufacturing,6 composite materials, electronic high dispersion in the surface area of composites and cast-
industry,7 fuel cell technology, nano materials,8 9 and bio ing defects will be reduced when compared to macro level
ash particles. The synthesized material mainly consists
∗
Author to whom correspondence should be addressed. of low density elevated hard ceramic particles. It is then

J. Nanosci. Nanotechnol. 2019, Vol. 19, No. 7 1533-4880/2019/19/4123/006 doi:10.1166/jnn.2019.16299 4123

Synthesis and Characterization of Coconut Shell Ash Satheesh et al.

reinforced with matrix material to increase the strength, 3. RESULTS AND DISCUSSION
wear resistance and also to reduce the density and weight 3.1. pH Measurement
of the fabricated composites.13 The application of nano The pH value of CSA was measured by digital pH meter
sized ash particles makes light weight and stronger struc- (Fig. 2) as per ASTM standard 3838-80. 1 gm sample
tural composite materials. The main objective of this work was added in 100 ml double distilled water. The mixture
is to focus on the utilization of extensively available agro was stirred at measured temperature 35.2  C till the con-
waste CSA in a useful manner by adding it to the alu- stant pH occurred. The pH value is measured by digital
minium alloy to produce aluminium hybrid composites by pH meter and value obtained is 7.47. These values indi-
stir casting method. cated that the CSA particles having base and not present
acid and alkaline materials.
2. EXPERIMENTAL DETAILS
3.2. Ash Content
Dry coconut shells were gathered from the nearby agricul-
tural area, oil mills and food production places. In order Ash content (quantity) of CSA was studied by heating ash
to remove the moisture content and dirt, the shells were at 800  C for 1 hour using muffle furnace. 1 gm of sam-
cleaned and sun dried for two to three days. The dried ple was taken in a silica crucible and it is heated upto
to 800  C in a furnace. During this process, the crucible
coconut shells were pulverized to powder form and placed
is kept open. After the required heating, the crucible is
in graphite crucible, then burned in open air till the powder
cooled in desiccators and the weight of ash is measured
gets complete combustion. After the complete combustion
by a digital weighing machine. The following equation is
in the open hearth, the coconut shell ash powders were
used to find the ash content presents in CSA particle.
allowed to hearth cooling at room temperature, before the
removal of CSA from crucible to avoid the formation of M − M1
% Ash content = 3 × 100 (1)
charcoal. M2 − M1
Figures 1(a) and (b) show the formation of coconut Where, M1 —Mass of empty crucible (gm), M2 —Crucible
shells powder and coconut shell ash powder. After success- with a mass of ash (gm), M3 —Crucible with dried a mass
ful completion of synthesizing the CSA, different charac- of ash (gm).
terization test has been done on CSA. Physical properties By using the above equation, percentage of ash content
such as pH value, density, ash content, moisture content,
IP: 5.189.201.171 On: Mon,present
18 Marin2019
CSA07:12:08
is 68.5% which shows that the quantity
loss on ignition, a grain size of CSA and surface
Copyright: area Scientific
American of ash isPublishers
typical one when compared with other research
including pore volume, pore size of CSA wereDelivered studied byworks.
Ingenta
by corresponding testing methods as per standard mea-
surement techniques. Chemical characterization study was 3.3. Moisture Content
carried out for chemical composition analysis, the mor- Moisture content is studied as per standard procedure.14
phology of ash particles, percentage of various elements It is analyzed by heating CSA to 105 ± 5  C for 1 hour in
present and various chemical functional groups present in the furnace and cooled to room temperature in desiccators.
the samples through XRF, SEM/EDS and FTIR techniques Dried samples were weighed and calculated by the below
respectively. Crystallite structures, average particle size, equation.
and thermal stability of CSA were investigated by XRD M − M2
hm = 1 × 100 (2)
and TGA methods. M2

(a) (b)

Figure 1. (a) Coconut shell powder (b) coconut shell ash.

4124 J. Nanosci. Nanotechnol. 19, 4123–4128, 2019

Satheesh et al. Synthesis and Characterization of Coconut Shell Ash

3.6. Grain Size Analysis

The Crystallite size analysis of the coconut shell ash par-
ticles was determined by using Scherrer’s formula17 with
help of XRD peak position data and FWHM.

Crystallite size D = k/B cos 

Where, D—average crystallite size (nm), k—Scherrer con-

stant (k varies from 0.68 to 2.08), (k = 0.98 for spherical
crystallite with cubic symmetry), —X-ray wave length,
Figure 2. pH measurement setup. B—FWHM (full width at half maximum), —XRD peak
position.
Where, M1 —Initial Mass of the sample (gm), M2 —Final The average crystallite size for CSA is 41.50 nm.
mass of dried ash (gm). The Crystallite size of CSA was found to be min
The moisture content present in CSA is 0.609% which 21.80 m, mean 41.50 nm and max 94.81 nm.
is determined by the above equation according to the
standard procedure. The result shows that the CSA par- 3.7. BET Analysis
ticles reinforcing with composites, does not absorb water BET analysis including surface area, pore volume, pore
or moisture particles, so as to avoid the corrosion of the size was studied at CSIR-NML Unit-Chennai. From the
components. result the specific BET surface area of the CSA was
found to be 175.0777 m2 /g, (whereas the coal fly ash
3.4. Loss on Ignition 122.1 m2 /g)18 average pore diameter of 4.479 nm. The
Loss on ignition is studied as per standard procedure by total pore volume for pores less than 164.529 nm is
heating the CSA to 975 ± 25  C for 1 hr and cooled in 0.0908 cm3 /g.
desiccators and weighed the samples.14
M1 − M2 3.8. SEM/EDS
Hm = × 100
IP: 5.189.201.171 On:(3)Mon,Microstructure
18 Mar 2019 07:12:08
evaluation and elemental analyses were
M1
Copyright: American Scientific Publishers
studied using SEM-EDS at IIT-Madras. The morpholo-
Where, M1 —Initial mass of ash (gm), M2 —FinalDelivered
mass of bygies
Ingenta
of the CSA particle and the composites by SEM with
dried ash (gm). EDS are shown in Figures 3(a), (b). CSA particles were
By using above equation the % of LOI present in CSA observed in irregular size and spherical shape particles can
is 11.5%. also be observed in the Figure 3(a). This spherical and
irregular shape helps to improve the bonding between the
3.5. Density Measurement particles and it reduces the gap between the matrix and
The power density of CSA was measured based on reinforcement particles. The chemical analysis of the CSA
ISO 8962 using a glass pycnometer and to determine true consists Si, C, O, Mg, Al with small amounts of Fe, Ca,
density.4 The density of CSA was determined by using the K, S, Na also presents in CSA as shown in Figure 3(b).
below equation.
mass 3.9. X-ray Fluorescence (XRF)
True density CSA = Chemical composition of CSA was analyzed by XRF
volume
(XGT-5200 X-ray analytical microscope, Horiba, Japan)
M3 − M1 
CSA = (4) technique at CECRI-Karaikudi and the composition of
M3 − M1 + M2 − M4  CSA as given in Table I. XRF is used to find out the ele-
Where, M1 —mass of dried empty pycnometer (gm), M2 — mental composition which is present in CSA. The result
mass of pycnometer with distilled water (gm), M3 — shows that the highest compound of CSA is SiO2 . How-
mass of dried pycnometer with CSA (gm), M4 —mass ever, CSA is hard because it contains high percentage of
of pycnometer containing CSA and filled with distilled SiO2 , Al2 O3 , and Fe2 O3 which are acknowledged through
water (gm). among the strongest materials.
By using the above equations, the calculated density Moreover, SiO2 is about 65% which is similar value
value of CSA is 1.65 g/cc. It shows that the CSA has low achieved by Stanislav et al.10 and the combined mass%
density and it can be used in aluminium matrix composites of SiO2 , Al2 O3 , Fe2 O3 is around 85% which will help to
to reduce the weight of the composite components. The increase the strength in MMC when compared to RHA
density of CSA value is low when compared to fly ash and (90% SiO2 , because it still weaker than CSA due to low
bagasse which is 2 to 2.5 and 1.95 g/cc respectively.15 16 percentage of Al2 O3 , (1.32) and Fe2 O3 (1.43).2

J. Nanosci. Nanotechnol. 19, 4123–4128, 2019 4125

Synthesis and Characterization of Coconut Shell Ash Satheesh et al.

Figure 4. XRD analysis of coconut shell ash.

SiO2 and Al2 O3 are well known reinforcing additives for

improving wear resistance.20

3.11. FT-IR
A FTIR Fourier transform infrared spectrophotometer
(SHIMADZU) was used to study the functional groups
present in the coconut shell ash FTIR (Model-FT/
IR-4700typeA, at CSIR-CLRI-Chennai. The qualitative
analysis of coconut shell ash was analyzed by the
IP: 5.189.201.171 On: Mon,FT-IR 18 Mar 2019 measurements
spectral 07:12:08 were depicted in Figure 5.
Figure 3. (a) SEM image of CSA and (b) EDAX analyses. American Scientific
Copyright: Publishers
The FT-IR
Delivered by Ingenta spectra were recorded in the range of
400 cm−1 –4000 cm−1 respectively. Five main bands are
3.10. X-ray Diffraction Analysis
seen in Figure 5. The peak at 3185 cm−1 was due to O–H
An identification of unknown crystalline materials, vari-
stretching mode of vibration and appearing peaks in the
ous functional groups present in the element of CSA was
range of 2804 cm−1 was due to C–H stretching vibra-
analyzed by using Powder XRD, methods at CSIR-CLRI-
tions. The broad peak observed at 1057 cm−1 was due to
Chennai. The samples were exposed to X-ray genera-
the stretching mode of vibration of C–O respectively. The
tor running at 30 kv. The 2 angle for the machine
band at 775 cm−1 was attributed to C–H in benzene rings
ranges from 3 –80 with a sampling step of 0.005 at a
and aromatic ring, the observed FT-IR spectral measure-
scan speed of 4 deg/min were employed. Crystallite size
ments indicates the presence of ash.
was calculated using XRD result by means of scherrer’s
equation.
3.12. Thermo Gravimetric Analysis (TGA)
The crystal structures of coconut shell ash were inves-
tigated by X-ray diffraction (XRD) as shown in the The thermal behavior of ash was studied by the Thermo
Table II. The XRD technique is used and the presence Gravimetric (TG) analysis. The TGA for ash has been
of SiO2 , Al2 O3 , Fe2 O3 was found as shown in Figure 4.
The predominant peaks SiO2 observed at 26.69 which is Table II. Structural properties of coconut shell ash.
in good agreement with the JCPDS data 00-001-0649.19 S. no. Peak position 2 ( ) FWHM (B) Crystallite size (D)
Quartz is the major component contributed to crystalline
phase formed in the sample. The oxides like SiO2 , Al2 O3 1 20.84 0.22 38.38
2 26.69 0.18 47.45
and Fe2 O3 make the matrix harder and more durable 3 35.56 0.44 21.80
which results in improved physical-mechanical properties. 4 39.45 0.16 55.13
5 42.46 0.34 26.20
6 45.86 0.23 39.30
Table I. Chemical composition of CSA.
7 50.16 0.13 68.93
Elements SiO2 Al2 O3 Fe2 O3 CaO K2 O TiO2 8 54.88 0.17 55.04
9 59.92 0.24 41.66
Mass% 65.874 4.778 14.225 5.773 8.998 0.323 10 68.29 0.46 21.81

4126 J. Nanosci. Nanotechnol. 19, 4123–4128, 2019

Satheesh et al. Synthesis and Characterization of Coconut Shell Ash

Figure 5. FT-IR spectra of coconut shell ash.

recorded using TGA Q50 V20.5 Build 30 Instrument at 4. CONCLUSION

CSIR-CLRI-Chennai. Alumina crucible was used for heat- Synthesizing of CSA was successfully made and their
ing the sample. physical and chemical characterizations were analyzed.
The Thermo Gravimetric Analysis (TGA) of CSA was In this experimental investigation, it is observed that the
carried out an the sample weight of 14.3160 mg between coconut shell ash is very strong than the rice husk ash
room temperature to 800  C at a heating rate of 20  C/min and palm kernel shell ash based on XRF properties. The
in nitrogen atmosphere and the resulting thermogram is true density of CSA is low (1.65 g/cc) when compared
shown in Figure 6. From the TG curve, it is obvious to fly ash and bagasse ash and it can be used as a filler
that the material is stable and there is no phase transi- material for making low density AMC materials. This fab-
tion upto 87.27  C. But mass lossIP:
upto 87.27  C is 0.68%
5.189.201.171 On: Mon,rication
18 Marmethod
2019 07:12:08
gives higher ash content (68.5%) with low
due to the presence of moisture content Copyright:
in CSA American
parti- Scientific
moisture Publishers
content (0.609%) and loss on ignition is low as
cles. The loss of weight in the region betweenDelivered
335.20 by11.5%
Ingenta
for CSA particles. The average particle size of CSA

and 534.59 C (0.38%) may be due to the elimination of is 41.5 nm obtained from XRD using Scherrer’s formula.
Al and Si species when the testing parameters affect the Thus the porosity of composite materials can be mini-
mass loss recorded at temperature relevant 700–1000  C mized. The specific BET surface area of the CSA col-
of ashes, mainly associated with oxidation reaction taking lected from the open fire was found as 175.0777 m2 /g,
place upon heating.21 22 average pore diameter of 4.479 nm. The total pore vol-
ume for pores less than 164.529 nm is 0.0908 cm3 /g.
Hence it is found that the increasing surface area per unit
100.0 weight of CSA particles can be dispersed uniformly in
87.27 °C the matrix (aluminium). XRF and XRD studies discovered
99.28 % the presence of hard particles like SiO2 , Al2 O3 , Fe2 O3 as
99.5
major constituents which can be used as particulate rein-
forcements in MMCs for making Aluminium Composites.
FTIR graphs showed that O–H, C–H and C–O phases were
Weight (%)

99.0
335.20 °C
98.70% present in CSA and proposed to use CSA as particulate
reinforcement in MMCs.
98.5 534.59 °C
98.32%
.
References and Notes
Residue:
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Received: 1 May 2018. Accepted: 20 June 2018.

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