Chapter three

Materials and methodology

3.1 materials
A low cost manufacturing process using simple experimental
design methodology has been developed for this study, and no
expensive machinery was required for processing. Locally evaluable
raw materials were used in this work.
The agro-waste material (cassava cortex) was obtained from
local markets in Nsukka in Enugu state. Simple molding process was
used in the sample fabrication. After the fabrication of the samples,
they were subjected to series of tests such as dielectric test and
mechanical tests. The description of the process is shown below.

3.2 Experimental Materials

I.
II.
III.

Cassava cortex
Epoxy resin
Hardener

Cassava cortex: cassava cortex is the raw material that constitutes

the particulate of the composite. It is gotten by peeling off the back of
a cassava and allowing it to dry in the sun. This material forms a
composite with good dielectric property when mixed with epoxy.
Epoxy resin: Epoxy belongs to a class of polymer called thermoset. It
is hard, tough, insoluble and infusible when cured. Its property of
infusibility differentiates thermoset from thermoplastics. Epoxy cure at
room temperature. During curing, it undergo exothermic reaction.
Epoxy is the most widely used polymer because of its exceptional
properties. Below are the advantages one can gain from using epoxy
resin:

1.
2.
3.
4.
5.
6.
7.
8.
9.

Good handling characteristic.

Low shrinkage.
Excellent adhesive property.
Flame resistance.
Good chemical resistance.
No by-product form during curing.
Good mechanical properties.
Good electrical resistivity.
Good dielectric constant.

Hardener:

these

are

comprehensive

line

of

anhydride

based

hardeners designed for indoor/outdoor electrical application and

composites. When paired with a compactible epoxy resin, anhydride
based polymers offers low viscosity, UV stability, high temperature
performance and good electrical insulation properties.

3.2.1 Preparation of cassava cortex

The cassava peels used was sourced locally from markets in
Nsukka in Enugu state. The cassava peels was sun dried after which,
the brown exterior of the cassava peel was easily removed with hand.
Part of the cassava cortex was carbonized and some of them was left
uncarbonized. For the carbonized cassava cortex, the carbonization
was done at a temperature of 300 degree Celsius. The cortex was
ground into powder using grinding machine. After the grinding, sieve
analysis was carried out on the particle. This is where different particle
size of the powder was separated using sieve. Particle size of
150microns, 300microns and 600microns where used. The cassava
cortex powder which is now the reinforcement was mixed with epoxy
gum which is the matrix in certain ratio that will be later specified and
stirred, after which, the mixture will now be cast into the mold for the
fabrication into any desired shape. After the casting, the specimen was
allowed to dry and solidify.

3.3 fabrication process

A relatively low cost polymer composite manufacturing process
using simple experimental design methodology was employed for this
study. The activities involved are classified into three steps, which
include:

Molding making
Preparation of the composition for the samples
Casting

3.3.1 Molding making

The materials used for the preparation of the molds is an
embossed paper. This embossed paper is cut into different sizes and
shapes for the fabrication of the mold. After the mold has been
fabricated, they were placed on a flat metal sheet and with masking
tape, these molds where held in place. For the cylindrical molds, it was
ensured that the base of the mold was firmly held to avoid leakage
during pouring.
3.3.2 Preparation of the composite for the samples
S/N
1

Designation
Composition
150 microns cassava 40% epoxy + 20% hardener + 40%
cortex particulate

particulate
33% epoxy + 17% hardener + 50%
particulate
27% epoxy + 13% hardener + 60%

particulate
300 microns cassava 40% epoxy + 20% hardener + 40%
cortex particulate

particulate
33% epoxy + 17% hardener + 50%
particulate
27% epoxy + 13% hardener + 60%
particulate

600 microns cassava 40% epoxy + 20% hardener + 40%

cortex particulate

particulate
33% epoxy + 17% hardener + 50%
particulate
27% epoxy + 13% hardener + 60%
particulate

From the table above, samples were produced for each particulate size.
3.3.3 Casting of the samples
The casting process is the last stage of fabrication of the sample.
After the equivalent volume is known for each sample, releasing agent
was properly applied in the mold for easy removal of the sample after
curing. The resin (epoxy) is then mixed with the hardener in the ratio of
2:1 in a glass beaker and stirred properly. The particulate was then
measured and poured into the mixture, it was stirred to ensure a
homogeneous mixture. After the stirring, it was poured into the mold
and allowed to cure. After curing, the samples were removed from the
mold and were taken to the next procedure which involved testing.

3.4 Testing of fabricated samples

The tests that were carried out on these samples are for the
determination

of

the

breakdown

voltage,

dielectric

test,

water

absorption capacity test, moisture content test, surface resistivity and

volume resistivity, mechanical testing which include tensile test,
compressive test, flexural test, impact test, hardness test and wear
test.
3.4.1 Breakdown voltage

The cylindrical sample of 25mm diameter and thickness of 5mm was placed
between two sphere-type electrodes of 20mm diameter and an impulse voltage was
gradually applied to the sample from the control desk. The value at which the insulator
failed is recorded and the breakdown voltage of all the specimen is recorded via the same
procedure.

3.4.2 Dielectric test

To determine the dielectric constant, the composite samples
were molded into rectangular plates of length 50mm, width 30mm and
thickness 2mm. the figure below shows the plan for the experimental
setup used for the determination of the dielectric constant. It
comprises of two parallel plate capacitors, DC battery, and a digital
multimeter for measuring the applied voltage across the samples. An
air gap was created between two parallel plate capacitors which has
the same thickness with the sample. The parallel plate capacitors were
connected to the battery and the voltage across was measured (Vo).
The samples were then inserted between this air gap and the different
voltage was taken for the different samples.
Given below is the relationship between the Vo (voltage between the
capacitor with an air gap between them) and V (voltage across the
capacitor with the sample between them).
Below is the diagram of the dielectric test being perform.

3.4.3 Water absorption capacity test

The water absorbed by the material is specified as the
percentage weight gained by the material. With the cylindrical sample
of length 30mm and diameter 15mm, the samples were weight to the
nearest 0.01g (M1) and immersed in the water for a period of one
month (30 days) after which, it was removed from the water and
allowed to drain in the ambient, then the sample was weighed again
the second time (M2). The water absorbed was calculated as
percentage weight gain using the following formula:

Wa=

( M 2M 1 )
100
M1

3.4.4 Moisture content

The moisture present in the samples has samples has significant
effects on the dielectric strength and resistivity of the materials. Therefore,
the moisture content at the time of measurement is needed to be specified.
The sample with length 5mm and diameter 15mm was taken and each of
them was weighed to the nearest 0.01g (M3), the samples were then placed
in an oven for 3 hours at 90 degree Celsius. After proper drying, the samples
were weighed to obtain the value (M4). The moisture content was calculated
as percentage of the dry sample using the following equation:
Wc=

( M 3M 4 )
100
M3

3.4.5 Tensile test

The strength of the insulators was investigated by determining their tensile strength
according to (ASTM, 1985b). A Universal tensile testing machine was used to carry out
the failing load of the samples. The insulators were coupled on the tensile machine and
allowed to be loaded up to until failure was experienced.

3.4.6 Impact test

3.4.7 Linear Shrinkage

The dimensional changes in length were taken and the results were used to determine the
linear shrinkage after firing at 105C. The linear shrinkage was determined using
equations (1) to (3) below.

Drying shrinkage =

LwLd
100
Ld

Fired shrinkage =

LwLf
100
Ld

(2)

Total shrinkage =

LwLf
100
Lw

(3)

(1)

Where Ld = Dry length, Lw = Wet length, Lf = Fired length

3.4.8 Density
Density was calculated using a direct volume measurement method. This method
involves the use of water displacement method and the mass of the samples. The mass of
the sample divided by the volume of the displaced water will give the density of the
samples

Density =

M
v =mass/volume (g/cm3)

Chapter 4
Data, analysis and interpretation
This chapter is centered on the explanation of all the results of the
tests that has been carried out on the fabricated sample. Some of these tests
are destructive (damaging the specimen after the test) while some of them
are non-destructive (the specimen still intact after the test was conducted)

Below are the data generated for the various tests and the possible
explanations to the nature of the prevailing values
4.1 breakdown voltage.
Below is the breakdown voltage value of the composite with different volume
fraction of particles and epoxy
S/N
1
2
3
4
5
6
7
8
9
10

Sample
40% 150U
50% 150U
60% 150U
40% 300U
50% 300U
60% 300U
40% 600U
50% 600U
60% 600U
CONTROL

Breakdown voltage (V)

30
37
36
25
35
25
40
38
40

4.2 dielectric test

Below is the values gotten for the dielectric test conducted on the samples
S/N

Sample

Vo

across
1
2
3
4
5
6
7
8
9
10

40% 150U
50% 150U
60% 150U
40% 300U
50% 300U
60% 300U
40% 600U
50% 600U
60% 600U
control

air gap
1.00059
1.00059
1.00059
1.00059
1.00059
1.00059
1.00059
1.00059
1.00059
1.00059

voltage V
with

voltage

an across with the

sample
1.02V
0.06V
0.10V
0.65V
1.15V
0.20V
0.10V
0.21V
0.20V

Vo
V

0.9810
16.6765
10.0059
1.5394
0.8701
5.0030
10.0059
4.7647
5.0030

4.3 water absorption capacity test

Below are the values gotten form the test conducted on water absorption
capacity of the samples
S/

Samples

Initial

weight Final

before
immersion

after
in from

weight Water

absorption

removal rate (%) WA=(M2water

= M1)/M1 X 100

40%

water = M1(g)
36

M2(g)
36

(percentage)
0

150U
50%

34

34

150U
60%

36

36

150U
40%

37

37

300U
50%

35

35

300U
60%

38

38

300U
40%

35

35

600U
50%

33

33

600U
60%

30

31

3.33

10

600U
control

37

37

From the table above, it can be observed that the composite has a zero
moisture absorption content. That is, the weight of the material before the
absorption is the weight of the material after the absorption.

4.4 moisture content

Below are the value gotten from the different samples based on the moisture
content test
S/

Samples

Initial weight Final

with moisture after drying in (%)

content

1
2
3
4
5
6
7
8
9
10

weight Moisture content

40% 150U
50% 150U
60% 150U
40% 300U
50% 300U
60% 300U
40% 600U
50% 600U
60% 600U
control

M3(g)
36
34
36
37
35
38
35
33
30
37

= the

oven

M4(g)
35
33
35
35
33
35
32
30
27
38

MC=(M3-

= M4)/M3 X 100
2.86
2.94
2.86
2.70
5.71
7.89
8.57
9.09
10.00
2.70

4.5 tensile test

The strength of the insulators was investigated with the help of the result. It was observed that the sample
with higher percentage composition of cassava has lower strength compared to the ones with high epoxy
content. This shows that the strength of the composite insulator are enhanced by the presence of the epoxy
matrix.

4.6 impact test

These are the values gotten from the impact test

S/N
1
2
3
4
5
6
7
8
9
10

Samples
40% 150U
50% 150U
60% 150U
40% 300U
50% 300U
60% 300U
40% 600U
50% 600U
60% 600U
CONTROL

Energy(J)
5.10
5.00
5.00
3.45
3.50
3.40
3.35
3.75
2.95
5.50

4.7 Linear Shrinkage

The total linear shrinkage percentage of insulators were found to increase with increasing
cassava cortex content and reduction of epoxy as indicated by Tables

S/N

Sample

Dry

Wet

Fired

Dry

Fired

Total

length

length

length

shrinka

shrinka

shrinka

ge
4.17

ge
4.17

40%

12

12

11.5

ge
0

150U
50%

12

12

11.1

7.50

7.50

150U
60%

12

12

10.9

9.16

9.17

150U
40%

12

12

10.4

13.33

13.33

300U
50%

12

12

10.5

12.50

12.50

300U
60%

12

12

10.0

16.67

16.67

300U
40%

12

12

9.80

18.33

18.33

600U
50%

12

12

9.80

18.33

18.33

600U
60%

12

12

9.70

19.67

19.17

600U

10

CONTROL

12

12

11.5

4.17

4.17

4.8 Density
These are the values of density of the different samples of the composite.
S/N
1
2
3
4
5
6
7
8
9
10

Sample
40% 150U
50% 150U
60% 150U
40% 300U
50% 300U
60% 300U
40% 600U
50% 600U
60% 600U
CONTROL

Mass(g)

Volume(cm

Density(g/c

36
34
36
37
35
38
35
33
30
37

3)
25
25
27
24
28
29
30
26
27
27

m3)
1.44
1.36
1.33
1.54
1.25
1.31
1.17
1.27
1.11
1.37