The Synthesis of Graphene from Coconut Shell Charcoal

Minto Supeno*, Rikson Siburian, Desi Natalia

Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Sumatera Utara

Keywords: charcoal, sp

orbital, graphene, activated carbon, pyrolysis, coconut shell

Abstract: The hybrid coconut shell charcoal is sp

, after being mixed with activated carbon and heated to 600 for 1

hour it produces sp

which shows the characterization of graphene. The process of making graphene in this

study, namely coconut shell dried under sunlight then hydrolyzed into charcoal then mixed with activated

carbon as a reducing agent at 600°C for 1 hour to produce graphene. The resulting graphene is characterized

by XRD, SEM-EDX, XRF and BET. The results of the XRD analysis showed that the resulting peaks were

not sharp and slightly broadened the diffraction peak at 24° and 44°. The results of SEM-EDX analysis at

4000x magnification showed smaller, thinner surface sizes and structural shapes and reduced buildup in the

graphene structure. XRF analysis results show that there are still organic impurities. The results of graphene

analysis with BET show the surface area of graphene 82.873 m

/ g with a pore volume of 0.116 cc / g.

1 INTRODUCTION

Coconut shell is a hard part on coconut which

has a thickness between 3-8 mm which consists

mostly of lignin, cellulose, and hemicellulose.

Coconut shells can be converted into charcoal or

activated carbon through the carbonization process.

Coconut shell can be used as a carbon source in

graphene synthesis (Liyanage and Pieris, 2015).

Now, the most popular method for producing

single-layered and multi- layered graphene is by

solving methods or known as mechanical and

chemical methods. For the mechanical method, the

graphene produced is single layered. However, the

cost needed in making graphene is very expensive,

and graphene is produced in small quantities.

Meanwhile, with the chemical method, graphene

produced in large quantities and the preparation of

graphene is very simple, but the graphene produced is

still not single-layered (Siburian, 2012).

In general, graphene is made through the Hummer

method and got from graphite mining which comes

from nature and is a non-renewable resource.

Previous researchers were done by Supeno and

Siburian (2018) using coconut shells which were

converted into graphite and graphene nano switching.

The conversion of coconut shell into graphene can be

seen from the comparison of Aluminum-vessel effect

and Pyrex-Glass effect on the cracking process. On

Pyrex-Glass vessels the process of pyrolysis at high

temperatures will less contribute in donating

electrons to the coconut shell compared to the

Aluminum-vessel vessel and then continued

pyrolysis at a temperature of 600°C. Previous

researchers assumed that coconut plants were an

abundant natural resource and the constituent carbon

was C-amorphous. Therefore, through this research

coconut shell was used as a carbon source in graphene

synthesis. Graphene synthesis starts from carbonize

coconut shell into charcoal. After the coconut shell

structure changed from physical structure to charcoal,

then the reducing agent is activated carbon is added

which functions to absorb the oxide present in the

charcoal with a temperature of 600°C which is

expected to synthesize graphene from coconut shell

charcoal. Based on the background described, it is

necessary to do some research with the title "The

Synthesis of Graphene from Coconut Shell

Charcoal".

Supeno, M., Siburian, R. and Natalia, D.

The Synthesis of Graphene from Coconut Shell Charcoal.

DOI: 10.5220/0008839600390044

In Proceedings of the 1st International Conference on Chemical Science and Technology Innovation (ICOCSTI 2019), pages 39-44

ISBN: 978-989-758-415-2

2 MATERIALS AND METHODS

2.1 Tools

Tools used in this experiment: Glassware, Analytical

Balance, Tube Clamp, Watch Glass, Porcelain Saucer,

Filter Paper, Mortar, Funnel, Magnetic Bar,

Furnace, 100 mesh sieve, 150 mesh sieve, Oven,

Spatula, Electron Scanning Microscope, X-Ray

Diffraction, Brunauer–Emmet– Teller, Fluorescence

Spectroscopy X-ray.

2.2 Materials

Materials used in this experiment: coconut shell,

activated carbon, aquadest and KOH 1 N.

2.3 Procedure

2.3.1 Making of Charcoal

Coconut shells are dried in the sun until dry. Then, 1

kg of coconut shell is taken, then hydrolyzed in the

furnace in an oxygen free condition for 5 hours at

600°C until became charcoal. Smoothed using

mortar. Furthermore, it is shifted using a 100-mesh

size sieve. Then, it was characterized using XRD and

SEM.

2.3.2 Synthesis of Graphene

Charcoal from the coconut shell is in chip form, then

weighed as much as 15 g and mixed with activated

carbon powder. Then it was heated at 600°C for 1

hour. Then sifted using 150 mesh sieves. Coconut

shells are washed with distilled water until clean, and

dried in an oven at 70°C. Furthermore, it was

characterized using XRD, XRF, SEM-EDX, and

BET.

2.3.3 Effect of Addition of KOH 1 N Solution

on Surface Area and Graphene Pore

Size

Weighed 15 g of graphene and then soaked with KOH

1 N for 2 hours. Then precipitated in the oven for 1 h

until dry. Furthermore, the graphene is heated in a

furnace at 600°C for 1 hour. Furthermore, it was

characterized by using XRD and BET.

3 RESULTS AND DISCUSSIONS

3.1 Making of Charcoal

Coconut shells are cleaned then the coconut

shell is burned at 600°C for 5 hours until it turns black

and turns into charcoal. According to Liyanage and

Pieris (2015) the heating process in the coconut shell

will produce gradual changes. Coconut shell charcoal

produced, mashed with a 100-mesh sieve. The

coconut shell charcoal powder produced was

characterized using XRD and SEM-EDX.

Figure 1: XRD diffractogram coconut shell charcoal

powder

The diffractogram showed by Figure.1, which is

XRD analysis shows that there are sharp peaks and

densities in several regions 2θ starting from 28°

diffraction angle which indicating that the phase

formed is the crystalline phase. The data obtained is

characteristic of the crystal structure of graphite

(Chen and Yan, 2009).

The results of the surface morphology scale

analysis by Scanning Electron Microscope (SEM) on

coconut shell charcoal powder with 4000x

magnification can be seen in Figure 2.

Figure 2: Surface morphology scale by scanning electron

microscope (SEM) on coconut shell charcoal powder with

4000x magnification

0 10203040506070

Intensity (a.u)

2 (



)

Coconut Shell Charcoal

C (002)

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SEM testing aimed to observe the surface

morphology and particle shape of the sample. At

4000x magnification, the coconut shell charcoal

powder in the form of piles showed that the coconut

shell charcoal powder had a layer structure.

3.2 Analysis of Graphene Powder

Structure from Coconut Shell

Charcoal

Graphene powder from coconut shell charcoal in this

experiment was produced from the pyrolysis of old

coconut shell by mixing activated carbon as a

reducing agent with a temperature of 600°C in the

furnace for 1 hour. The structure and phase analysis

of graphene from coconut shell charcoal used X-Ray

Diffraction (XRD), SEM-EDX, XRF and BET.

3.2.1 XRD Data Graphene Powder from

Coconut Shell Charcoal

Figure 3: XRD diffratogram graphene powder from

coconut shell charcoal

Diffraction peaks resulted are weaker and wider

indicating a reduction in some functional groups.

3.2.2 SEM-EDX Data Graphene Powder

from Coconut Shell Charcoal

The results of the surface morphology scale analysis

by Scanning Electron Microscope (SEM) analysis of

graphene powder from coconut shell charcoal with

4000x magnification can be seen in Figure 4.

Figure 4: Surface morphology scale by sem of graphene

powder from coconut shell charcoal with 4000x

magnification

Based on the results of SEM analysis, it is seen that

the formation of graphene layers piled on the 4000x

scale (Supeno and Siburian, 2018) was formed due to

the reduction of carbon on the surface of coconut shell

charcoal.

3.2.3 Analysis of Composite Graphene

Powder from Coconut Shell Charcoal

To analyze impurity phase and to determine the

composition of the elements contained in the material

used X- Ray Fluorescence (XRF) which can analyze

elements of Sodium to Uranium. However, testing

using XRF has not been able to measure the

percentage of the main content of graphene in the

form of C, H, O, N, and S because, it has a lower

atomic number than Sodium.

Coconut shell has a lot of lignin, so it is common

to find a lot of potassium content from the resulting

graphene powder. Other impurities such as Sulfur and

Phosphorus are natural materials which are also found

in natural materials such as coconut shells (Campbell,

2006).

3.2.4 Adsorption-Desorption Nitrogen

Isotherm Analysis of Graphene

Powder from Coconut Shell Charcoal

To measure porosity of mesopore graphene material

and pore size distribution, isotherm adsorption-

desorption of nitrogen is carried out. Graphic curve

adsorption-desorption of graphene powder with the

BJH method can be seen in Figure 5.

The Synthesis of Graphene from Coconut Shell Charcoal

Figure 5: Adsorption-desorption curve of graphene powder

by BJH method

Figure 5 showed type VI adsorption isotherm

according to the IUPAC classification. The non-

uniform surface of graphene to produce Type VI is a

very homogeneous and non-porous characteristic of

two-dimensional solids. To find out the graph of the

distribution of pore size and surface area adsorption,

the Barrett-Joyner-Halenda (BJH) method can be

seen in Figure 6.

Figure 6: Distribution of pore size and surface area

adsorption by Barret-Joyner-Halenda method

Based on Figure 6 graphene powder from coconut

shell charcoal absorbs nitrogen gas (adsorption

isotherm) on the surface of the sample at low

pressure. The results of adsorption- desorption

analysis of nitrogen powder gas graphene BJH

method produce the surface area and pore size shown

in Table 4.1

Table 1: The results of adsorption- desorption analysis of

nitrogen powder gas graphene BJH method

Adsorption-desorption

data

Graphene

Surface area 82.873 m

Pore volume 0.116 cc/g

Pore radius 1.8098 nm

3.3 Structure Analysis of Graphene

Powder from Coconut Shell

Charcoal by Adding KOH 1 N

Solution

Graphene powder from coconut shell charcoal with

the addition of 1 N. KOH solution. Analysis of the

structure and phase of graphene from coconut shell

charcoal using X-Ray Diffraction (XRD) and BET.

3.3.1 Analysis of XRD Graphene Powder

from Coconut Shell Charcoal by

Adding KOH 1 N Solution

The results of XRD diffraction analysis of graphene

powder from coconut shell charcoal can be seen in

Figure 7.

Figure 7: XRD from graphene powder with adding KOH 1

N from coconut shell charcoal

The resulting diffraction peak is at 24°. The resulting

diffraction peak is weak and wide which indicates

formation of graphene. The effect of adding KOH to

activate graphene produces a large surface area and

pore size.

3.3.2 Adsorption-desorption Nitrogen

Isotherm Analysis of Graphene

Powder from Coconut Shell Charcoal

byA KOH 1 N

To measure the porosity of mesopore graphene

material by adding KOH 1 N solution and pore size

0 200 400 600 800 1000 1200 1400

Pore Volume (cc/g)

Radius (Å)

Distribution of Pore Size and Surface Area Adsorption

10 20 30 40 50 60 70

Intensity (a.u)















Graphene+KOH 1N

C (002)

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distribution, adsorption-desorption nitrogen isotherm

analysis carried out. Potassium hydroxide as an

activator solution played an important role in yield

results. The presence of KOH during activation

results in degradation of the material that will form

the pore. Graphic curve adsorption-desorption of

graphene powder with the addition of KOH 1 N with

the BJH method can be seen in Figure 8.

Figure 8: Graphic curve adsorption-desorption of graphene

powder with the addition of KOH 1 N with the BJH

method

From Figure 8 showed type IV adsorption

isotherm according to IUPAC classification. From

the graph of adsorption-desorption of nitrogen

isotherm from graphene with the addition of KOH 1

N. The results showed that the porous material

subjected to nitrogen gas was included in the

mesoporous category. The results of gas

adsorption-desorption analysis nitrogen graphene

powder with the addition of KOH 1 N with the BJH

method produced the surface area and pore size

shown in Table 2

Table 2: The results of gas adsorption-desorption analysis

nitrogen graphene powder with the addition of KOH 1 N

with BJH method produced surface area and pore size

Adsorption-desorption Graphene

Surface area 40.494 m

Pore volume 0.060 cc/g

From Table 2, it can be concluded, in this

activation process carbon will react with KOH so

that carbon will be eroded (forming holes) resulting

in the formation of pores. In this experiment the pore

size and surface area were smaller than before the

addition of KOH 1 N, graphene surface area 82.873

/ g and the graphene pore size 1.8098 nm. The

researcher thinks this is because the concentration of

the activating solution is low and between the

substances reacting between the mixed substances

do not touch each other so that it produces a small

surface area and pore size (Erliana, 2015).

4 CONCLUSIONS

Based on the results of the experiment conducted, it

can be concluded as follows: Graphene can be

synthesized from coconut shell charcoal using

activated carbon as a reducing agent. The results of

characterization by XRD analysis showed

diffraction peaks at 24°. The results of SEM-EDX

analysis at 4000x magnification showed smaller,

thinner surface sizes and structural shapes and

reduced build-up in the graphene structure. XRF

analysis results showed that there are still organic

impurities. The results of graphene analysis with

BET showed the surface area of graphene 82.873

/g with a pore volume 0.116 cc/ g. Activated

carbon can reduce graphene oxide to graphene.

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