Characterization of Activated Carbon Derived from

Narra (Pterocarpus indicus) Wood Sawdust

as a Potential Electrode Material

A Research Proposal Presented to the

Senior High School Department of
Pasay City National Science High School
2888 Vergel Street, Pasay City

In Partial Fulfilment of the Requirements

for the subject Research in Daily Life 2

Presented by:
Medalla, Ana Maria Rachel B.
Paliza, Rai Jeriele C.
Torres, Nina Rhen Jasmine B.
Umila, Vhera Maye B.

G12 Zara

Presented to:
Mr. Christian Jayvon C. Laluna
Research Adviser

January 2024

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 CHAPTER 1
Introduction

The increasing economic development and population growth have caused a

significant energy demand (Nepal & Paija, 2019). Higher energy consumption,
primarily from finite resources such as fossil fuels, poses environmental problems
(Phainuphong et al., 2022), including increased greenhouse emissions and pollution
(United Nations, n.d.), making renewable energy a viable and environmentally
friendly alternative, with energy storage critical to its continuous supply
(Papathanasiou, 2023). In consideration of these, electrode materials play a significant
role in determining the performance and effectiveness of energy storage devices,
particularly in batteries and capacitors. Aside from any conductive materials,
electrode materials can also be derived from carbon-based materials and biomass
materials. Since wood is considered a biomass material and is used to turn into a
consumer product, the tonnage of wood and bark goes to waste in the Philippines
because of the inability of the logger or the manufacturer to find profitable uses for
these residues (Hunt, n.d.). According to Jabile et al. (2022), the Philippines generates
large amounts of wood sawdust as a by-product of sawmill operations. An example of
such wood commonly used in the Philippines is narra wood, which stores 87.81 Mg
C/ha carbon content (Pansit, 2019). In recent years, organic electrode materials have
gained interest due to their flexibility, low cost, lightweight, environmental
friendliness, and uses in various applications in architecture (Poizot et al., 2020). They
also stated that several issues and challenges associated with organic electrode
materials should be investigated and overcome. This includes material capacity,
device voltage, rate capability, and cycling stability. Thus, this study will explore a
new material—a Narra Wood Sawdust-Activated Carbon (NWS-AC) as a potential
electrode material.

Moreover, the Philippines is the second largest nickel producer, nickel as the
primary common electrode material (Ignacio, 2021). However, regardless of the
Philippines' status as a nickel producer, obtaining it causes drawbacks, hindering the
progression of safe and sustainable electrode production. The recent events in

1
Brooke's Point, Palawan, reveal that mining caused a heavy flood (MGB
MIMAROPA, 2023), demonstrating the detrimental effects of nickel extraction on the
local environment by exhibiting that the mine was the source of a significant flood.
For the country's need to harvest nickel to manufacture electrodes, mining deteriorates
the surrounding communities, disrupts local ecosystems, and damages natural
landscapes.

Additionally, according to Yan (2023), with the depletion of fuel supplies and
the rise in environmental pollutants, the need to develop efficient energy conversion
and storage technology is progressively growing. Therefore, fast-charging battery
technology is highly desired to fulfill the high power and long cycle life needs of
electric tools, such as supercapacitors and batteries, while also assisting in reducing
environmental pollution and advancing sustainable energy.

Furthermore, there has also been a rise in agricultural waste, specifically

sawdust, wood waste, or scrap, in the Philippines. The country has approximately 400
wood-processing facilities, with 355 sawmill enterprises, resulting in excessive
sawdust waste (Lantican, n.d.; Jabile et al., 2022). Consequently, this waste is often
left in landfills, exacerbating environmental concerns as it releases harmful chemicals
into the environment (Jan, 2022). Additionally, mounds of sawdust wood waste are
dispersed and burnt, resulting in poor thermal efficiency and further contributing to
air pollution and global warming (Jabile et al., 2022; Udokpoh & Nnaji, 2023).

With many issues regarding wood waste recycling and the advancement of
green electrode materials, this study aims to characterize and evaluate the thermal
resistivity and electrochemical performance of activated carbon derived from Narra
(Pterocarpus indicus) wood sawdust as a potential electrode material. One of the
requirements for activated carbon to become a potential electrode is for the variable to
have a high acquisition of carbon content; it was found by Pansit (2019) that Narra
has a carbon content of 87.81 Mg C/ha. Earlier studies have also shown that wood
sawdust can be a starting material for creating carbon-based electrode materials
(Maharjan et al., 2019; Phainuphong et al., 2022; Zhang et al., 2023). In a recent study
by Phainuphong et al. (2022), an electrode material made from activated carbon

2
derived from rubberwood sawdust exhibited exceptional electrochemical properties,
making it a promising candidate for supercapacitors.

Furthermore, electrode materials establish contact with a non-metallic part of a

circuit through which an electrical current passes (EDM Electrode Materials Selection
Guide: Types, Features, Applications | Engineering360, 2021). These materials are
widely used in various fields, such as chemical analysis, welding, cathodic protection,
and different types of batteries. Additionally, electrodes are used in medicine,
including ECG, ECT, EEG, defibrillator, and biomedical research through
electrophysiological methods (What Is Electrodes? - Types, Examples and Uses of
Electrodes, n.d.).

Electrode materials could play a vital role in several electronic tools and
storage, especially in areas with little to no access to energy. Thus, there is a need to
develop environmentally friendly and low-cost alternatives for a possible electrode
material. The application of sawdust waste as an electrode material could significantly
lower the rate of such waste in the country and provide crucial solutions and ways to
reduce the percentage of power- or energy-related issues. Moreover, the study's
success may also lead to further developments and widespread operations in the near
future.

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Statement of the Problem

The main problem in this study is to characterize activated carbon derived from
Narra (Pterocarpus indicus) wood sawdust as an electrode material.

Specifically, this study will answer the following:

1. What are the characteristics of the Narra Wood Sawdust-Charcoal

(NWS-Char) as an effective electrode in terms of:
1.1. Surface morphology; and
1.2. Elemental analysis?

2. What is the optimum carbonization temperature to produce the

Narra Wood Sawdust-Activated Carbon (NWS-AC) with optimum
quality in terms of:
2.1. 700°C;
2.2. 800°C; and
2.3. 900°C?

3. What is the electrochemical performance of the Narra Wood

Sawdust Activated Carbon (NWS-AC) as an electrode in terms of:
3.1. Thermogravimetric analysis (TGA); and
3.2. Cyclic Voltammetry (CV)?

4
Objectives

The study aims to characterize activated carbon derived from Narra

(Pterocarpus indicus) wood sawdust as an electrode material.

Specifically, the study aims to:

1. Identify the characteristics of the Narra Wood Sawdust-Charcoal

(NWS-Char) as an effective electrode material in terms of:
1.1. Surface morphology; and
1.2. Elemental analysis.

2. Determine the optimum carbonization temperature to produce the

Narra Wood Sawdust-Activated Carbon (NWS-AC) with optimum
quality in terms of:
2.1. 700°C;
2.2. 800°C; and
2.3. 900°C.

3. Assess the electrochemical performance of the Narra Wood

Sawdust-Activated Carbon (NWS-AC) as an electrode in terms of:
3.1. Thermogravimetric analysis (TGA); and
3.2. Cyclic Voltammetry (CV).

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Hypotheses

Null Hypothesis:
The Narra Wood Sawdust (NWS) activated carbon does not have the potential
to be an alternative electrode material.

Alternative Hypothesis:
The Narra Wood Sawdust (NWS) activated carbon has the potential to be an
alternative electrode material.

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Significance of the Study

Understanding sawdust’s performance as electrode material could lead to

cost-effective energy storage solutions, which might reduce the price due to its
relative abundance and increase the accessibility of energy storage devices (Gannett et
al., 2021). Further, this study also focuses on maintaining the continuous operation of
the electrode, decreasing the chance of people experiencing shorter usage times for
devices and, therefore, improving the performance of the devices. This may help
create efficient energy storage, which might benefit humanity by reducing the
environmental effects of energy storage technology and offering more sustainable
energy options (Shea & Luo, 2020).

This study will also benefit the community by exploring sustainable and
affordable materials for electrode materials from sawdust, contributing to the use of
waste materials in energy storage (Kayode & González, 2023). They also added that it
can enhance overall energy efficiency and reliability, meeting the energy demands of
the community. Likewise, this also provides an opportunity to lessen the usage of
fossil fuels in energy production, as it is considered the candidate to replace fossil
fuels due to its sustainability and low environmental impacts (Phainuphong et al.,
2022). It also reduces dependence on external resources as this study utilizes locally
accessible materials like sawdust and might offer localized energy solutions,
improving energy access for community members.

This study also holds significance to the world, as exploring biomass material,
like sawdust, as an electrode material offers a different approach and promotes waste
reduction (Chaudhari & Yu, 2019), reducing the quantity of waste produced
worldwide. Likewise, it lessens dependency on fossil fuels and advances a cleaner and
more sustainable energy environment. Additionally, this could improve global access
to energy as it can provide a versatile and affordable energy storage solution,
especially in areas lacking conventional energy infrastructure. Ultimately, this study
addresses the pressing challenges in the environment and limited resources and
embodies a joint effort towards sustainable and equitable energy for the entire world.

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Scope and Delimitation

This study primarily scopes on assessing the activated carbon derived from
Narra sawdust by investigating its physical and chemical characteristics through
Scanning Electron Microscope (SEM) and Energy Dispersive X-ray Spectroscopy
(EDX), thermal resistance through Thermogravimetric analysis (TGA), and
electrochemical current through Cyclic Voltammetry (CV). The evaluations will be
carried out at De La Salle University-Laguna (DLSU-Laguna), Advanced Device and
Materials Testing Laboratory (ADMATEL) of the Department of Science and
Technology (DOST), Adamson University (ADU) Chemistry Laboratory, and Pasay
City National Science High School (PCNSciHS) laboratories. The researchers will
only investigate the abovementioned properties of the activated carbon as they are the
crucial factors regarded most for potential electrode materials.

Moreover, the research will only focus on characterizing and determining the
electrochemical performance of NWS-Char and NWS-AC as an electrode. The study
will also only use surface morphology and elemental analysis as the testing methods
for NWS-Char. Likewise, testing methods such as thermogravimetric analysis (TGA)
and cyclic voltammetry (CV) are the only methods that will be used to assess the
electrochemical performance of NWS-AC as an electrode. Moreover, the
carbonization temperatures set in set-ups are 700°C, 800°C, and 900°C to produce
NWS-AC.

8
Definition of Terms

This study will characterize activated carbon derived from Narra (Pterocarpus
indicus) wood sawdust as an electrode material This study makes use of terminologies
that will be conceptually and operationally defined. The following terms will be used
within the context of the study.

Activated Carbon is charcoal that has undergone additional processing, such as

heating, to improve its adsorptive capacity.
Cyclic performance demonstrates the stability of discharge capacity and coulomb
efficiency. This is also greatly affected by the battery separators and will identify the
change in flow between the electrodes.
Electrochemical properties determine whether a separator is suitable for high-voltage
lithium-ion batteries.
Electrochemical Performance notably depends on the materials from which
electrocatalysts are formed, specifically on their surface area, catalytic activity,
electroconductivity, long-term stability, etc.
Electrode is a solid electric conductor that sends electricity into vacuums, plasmas,
gasses, non-metallic materials, and liquids.
Electrode Material is anything that can be utilized as an electrode.
Electrolytes are aqueous solutions that react exothermically with the cathode and
anode. This is observed to determine the change in the reaction between the anodes
and the cathodes.
Elemental Analysis is the process of determining the elemental and occasionally
isotopic composition of a sample of a material.
Morphological Characteristics are the properties observed in the composite
membranes that imply the transfer of lithium ions and the electrodes.
Thermal Efficiency is a system is the amount of work output for a given amount of
heat.
Thermogravimetric Analysis is a method where a sample specimen is exposed to a
controlled temperature program in a controlled atmosphere, and the mass of the
material is tracked as a function of temperature or time.

9
Porosity indicates an increase in advantage in terms of ionic transport and lessens the
polarization of the cell during the charge and discharge of the battery. This will be
observed to know the change in the polarization of cells when separators are used.

10
 CHAPTER 2
Review of Related Literature and Studies

This chapter presents the related literature and studies analyzed by the
researchers after a thorough and collective search. Diverse works of authors, both
local and international, were assimilated to formulate a solid background for the
current study. Only those that are considered relevant were studied.

Narra Wood Sawdust

Figure 1 Sawdust
Image source: https://www.linkedin.com/pulse/how-reuse-sawdust-issam-al-askary

Narra wood is widely distributed in South East Asia and South West Pacific
region (Kandasamy et al., 2021). They also stated that it had been commonly used
among artisans and builders for various applications such as furniture, light
construction, carving, and musical instruments. Although narra wood has sustainable
applications, it also produces an inevitable byproduct - sawdust waste - of the
wood/timber industry produced by cutting, sawing, or grinding timber (Martins et al.,
2022). However, rather than dismissing this byproduct as a waste, it holds untapped
potential as it is one of the most attractive biomaterials (Yasmin et al., 2021).

Narra wood sawdust emerges as a versatile byproduct, offering diverse

applications in different sectors and applications, including its role as a resource for
energy and environmental cleanup (Gavrilescu, 2020). With narra wood being a

11
biomass material containing 87.81 Mg C/ha carbon content (Pansit, 2019),
biomass-derived porous carbon materials have sparked significant interest among
researchers in terms of its energy storage applications due to their environmentally
friendly, abundant availability in nature, ease of fabrication process,
cost-effectiveness, and sustainable quality of the macro/meso/microporous carbon
generated from diverse biological precursors (Priya et al., 2023).

In relation to the study, sawdust from narra wood will be used to produce
charcoal derived from biomass material, particularly narra wood sawdust. It will then
undergo pyrolysis, producing activated carbon derived from narra wood sawdust as a
candidate for electrode material.

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Charcoal Derived from Narra Wood Sawdust

Figure 2 Sawdust Charcoal

Image source: https://www.google.com/amp/s/amp.abc.net.au/article/100741672

Charcoal is referred to as carbonized wood (Hagemann et al., 2018) that is

used for manufacturing activated carbon along with wood, nut shells, fruit pits, brown
and bituminous coals, lignite, peat, bone and paper mill waste (lignin), synthetic
polymers like PVC (Benitez et al., 2022). According to Rampe & Tiwow (2018), the
primary outcome of the pyrolysis process is charcoal with its by-products of liquid
smoke and tar. Furthermore, they also added that it comprises distinct constituents,
including bound carbon, water, ash, Nitrogen, and sulfur.

Charcoal has been used for various applications, and generating charcoal from
sawdust has been a popular solution for sawdust recycling (Lee, 2023). As
Ajimotokan et al. (2019) mentioned, carbonized wood is crucial for increasing
biomass use in electricity and heat production. They also stated that firewood, twigs,
and charcoal energy have been the primary renewable energy source for many
developing countries. In addition, charcoal from sawdust exemplifies the potential of
appropriate technology for wood waste utilization.

In a recent study by Phainuphong et al. (2022), results showed that

Rubberwood-Charcoal carbonized at 400°C exhibited a honeycomb-like structure
with pores when the samples were examined using the Field Emission Scanning
Electron Microscope (FESEM). The researchers found that increasing the KOH

13
impregnation ratio enhanced the charcoal's porous and well-structured surface.
Specifically, using a 1:3 ratio of KOH resulted in tiny pores at lower temperatures,
progressing to both small and medium-sized pores at higher temperatures. They added
that having these pores is crucial as it increases the surface area, making the charcoal
useful for creating efficient supercapacitors.

Concerning the study, NWS-Char is potentially processed into activated

carbon. Moreover, specific factors such as the surface morphology and elemental
composition will be considered.

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Pyrolysis

Figure 3 Pyrolysis Furnace

Image source: https://www.econ.eu/epo.html

Currently, there are multiple ways of creating AC, but this study will use
pyrolysis with potassium hydroxide chemical activation. Breaking down organic
material at a temperature without oxygen is called pyrolysis. When no oxygen is
present during pyrolysis, combustion cannot occur, retaining the carbonaceous
material and creating an extremely adsorptive compound (Amalina et al., 2022).
During pyrolysis, biomass is thermally broken down at temperatures ranging from
300°C to 1200°C. This process creates a carbon-rich substance and changes
complicated organic structures, setting the stage for the following activation step
(Zarei-Jelyani et al., 2023). The following activation procedure creates the porous
structure that characterizes activated carbon, and this precursor material serves as its
foundation (Saleem et al., 2019).

In recent studies, to obtain AC, biochar, a byproduct of biomass pyrolysis, is

used to make AC, which is necessary to unlock the material's full potential. The
activation process mainly involves Potassium Hydroxide (KOH). The porosity of the
biochar is increased by this activation phase, driving its specific surface areas to
remarkable 700–3000 m²/g ranges (Chen et al., 2020). Similarly to the study by
Zarei-Jelyani et al. (2023), the pyrolysis method was performed with the activation of
carbon. Also, the chemical activation with KOH resulted in the highest surface area
for wood-derived biochar. In addition to that, according to the methods of

15
Januszewicz et al. (2020), wood waste char was used as a potential material for
activating carbon. With the KOH as a chemical activator, the activation process was
heated at 850°C (heating rate of 10°C/min) under an N2 atmosphere (flow rate of 50
mL/min). As their results, 75% of activated carbon was obtained at wood waste char.

As a result, pyrolysis with the chemical activation of KOH is essential since it

is the first transformation that produces activating carbon, which establishes the
material's carbon-rich state, taking advantage of its activated carbon as an electrode
material.

16
Activated Carbon Derived from Narra Wood Sawdust

Figure 4 Sawdust Activated Carbon

Image source:
https://laoyingwendi.en.made-in-china.com/product/qwnTPtkoXWRO/China-Pyrolysis-Activated-Carbon-Black-P
owder-Pigment-for-Paint-Plant-Price.html

Environmental wastes that contain a lot of carbon are used to make activated
carbon. Peat, coal, nutshells, coconut shells, and wood are some of the raw resources
used to make it. It is possible to create AC from almost any carbon-heavy substance.
However, some are easier to get or yield a better-finished product (Omg, 2020).
Activated carbon is a cheap material with unique characteristics such as high porosity,
specific surface area, and specific surface functionalization. Activated carbon is
therefore utilized in many real-world applications such as adsorption, pollution
removal, water treatment, energy production, etc (Nile et al., 2022). Different methods
for preparing AC include pyrolysis, hydrothermal carbonization, and gasification
(Yaashikaa et al., 2020).

Activated carbon-based materials can be used for energy storage due to their
stated characteristics, such as their high surface area, high porosity, and conductivity.
These activated carbons have excellent electroactive properties, making them suitable
for supercapacitor electrodes and energy-storage devices (Nile et al., 2022).

According to recent studies, wood sawdust can be used as a starting material

to make carbon-based electrode materials. In a recent study by Phainuphong et al.
(2022), an electrode material composed of activated carbon produced from

17
rubberwood sawdust showed exceptional electrochemical characteristics, indicating
that it would be a viable choice for supercapacitors. Additionally, activated carbon
based on kara gash sawdust showed excellent high-rate capability and stable
cyclability, which made it a promising electrode material (Nazhipkyzy, 2022).

In reference to this study, narra sawdust will be utilized as activated carbon,

given that other studies used sawdust as activated carbon.

18
Surface Morphology and Elemental Characterization of Narra Wood
Sawdust-Char (NWS-Char)

Figure 5 SEM image of AC

Image source: https://www.mdpi.com/2073-4441/13/11/1453

Figure 6 EDX spectra of AC

Image source: https://www.mdpi.com/2073-4441/13/11/1453

Scanning Electron Microscopy (SEM) is designed to determine the surface

morphology of solids by utilizing a beam of concentrated electrons (Bradbury et al.,
2023). Specifically, SEM investigates the microstructure, sample homogeneity, pore
structure, and particle typography of the sample (Pallarès-Rusiñol et al., 2023).
Complementarily, Energy Dispersive X-ray Spectroscopy (EDX) is used to probe into
the char's elemental composition, which is vital for analyzing its organic contents and
their influences on the overall performance of the variable.

19
 Furthermore, utilizing SEM-EDX to assess the NWS-Char's surface
morphology enables a clearer understanding of its effectivity by closely observing the
Carbon (C), Oxygen (O), and Hydrogen (H); high carbon content and low oxygen
content, suggests a more effective biochar product (Gorrazzi et al., 2023).
Additionally, having a clear view of the NWS-Char pore structure is important to the
stability of the proposed activated carbon. It is expected that the char's surface is to
have balanced and abundant mesopores, macropores, and micropores (pores between
2 nm and 50 nm, greater than 50 nm, less than 2 nm, respectively in diameters) to be
considered highly stable and plausible as activated carbon for electrode materials
(Mendoza et al., 2022). Finding the optimal pore volume allows enlightenment
regarding the char's capacity to store electrolytes within its activated carbon structure.
Forbye the porosity, the AC shall also exhibit a uniform elemental distribution;
homogeneity of elements should be observed throughout the variable
(Pallarès-Rusiñol et al., 2023).

Overall, conducting SEM-EDX analysis is vital to investigate the sample's

structural integrity, significantly influencing the activated carbon's electrochemical
performance and thermal resistivity (SEM EDX Analysis | SEM Microscopy & SEM
Analysis, n.d.). Electrode materials should be observed to maintain a consistent
performance over multiple charge-discharge cycles; hence, studying its structural
characteristics is necessary (Yang et al., 2019).

20
Thermal Analysis of the Narra Wood Sawdust-Activated Carbon (NWS-AC)

Figure 7 TGA curves of AC

Image source:
https://www.researchgate.net/figure/Thermogravimetric-Analysis-TGA-of-biochar-and-activated-carbon_fig3_322
688119

Thermogravimetric analysis (TGA) is generally utilized to determine the

material's reaction to such temperature changes. Specifically, TGA assesses the
overall characteristics, including the variable's composition, purity, reactivity, and
thermal properties (Webdev, 2022). Moreover, the analysis is crucial in examining the
thermal resistivity of various energy storage tools (such as supercapacitors and
batteries).

Precisely, TGA is vital for evaluating the thermal behavior of the activated
carbon through a further investigation of its thermal stability, decomposition
characteristics, and optimal activation conditions to ensure reliable performance for
future applications on electrode materials. To be deemed reliable and effective, the
activated carbon should exhibit high thermal stability, resistance to high-temperature
breakdown, and minimal mass loss (Webdev, 2022). Furthermore, the graph indicates
the inverse proportionality of the object’s mass with temperature; the higher the
temperature is, the lower the mass should be; the lower the mass loss is at a changing
temperature indicates a thermally stable variable (De Fátima Salgado et al., 2018).

21
 Chiefly, TGA is a necessary technique to ensure a stable and efficient
operational functioning of the activated carbon derived from NWS. The interpretation
and data from the results shall apprise the effectivity and potential of NWS-AC as an
electrode material.

22
Cyclic Voltammetry Test of Narra Wood Sawdust-Activated Carbon (NWS-AC)

Figure 8 Cyclic Voltammogram of AC

Image:
source:https://www.researchgate.net/post/What_is_a_mechanism_and_real_meaning_of_quasi-rectangular_and_a
cute_triangle_shaped_cyclic_voltammetry_CV_curves_for_EDLC_type_carbon_materials

Cyclic Voltammetry (CV) is often used in electrochemistry to study redox

reactions by monitoring the current produced while adjusting the electrode voltage
(What Role Does Cyclic Voltammetry Play in Battery Testing? | Nanoscience
Instruments, 2023). CV is commonly used to study a chemical reaction's reversibility,
understand electron transfer kinetics, and estimate the energy levels of
semiconducting polymers. Moreover, CV provides valuable data such as anodic and
cathodic peak currents and potentials, the polarographic half-wave potential, and the
oxidation and reduction onset potentials. By analyzing this data, qualitative and
quantitative information about the electrochemical properties of chemicals can be
obtained. Additionally, CV can be used to identify the presence of a specific material
in a sample (Cyclic Voltammetry Uses | How to Read a Voltammogram, n.d.).

The graph showing the current and potential relationship is called a

voltammogram. Specific points, peak currents, and peak potentials are identified to
determine the oxidation and reduction reactions of the analyte. Additionally, the shape
and size of the peaks are used to estimate the electrochemical process's kinetics,

23
reversibility, and diffusion (What Is CV? A Comprehensive Guide to Cyclic
Voltammetry, n.d.; Cyclic Voltammetry, n.d.).

In the study, CV will be used to evaluate the electrochemical capacitance of

the NWS-AC. The cyclic voltammogram is expected to show a quasi-rectangular
shape, which suggests that the NWS-AC is a potential electrode that behaves like an
ideal capacitor (Phainuphong et al., 2022; Why Does an Ideal Capacitor Give Rise to
a Rectangular Cyclic Voltammogram (CV)?, n.d.).

Synthesis

To make use of the abundant Narra tree in the country (Kandasamy et al.,
2021), the NWS, which is a byproduct of various industries, will be utilized in the
study to reduce environmental waste (Gavrilescu, 2020). The study will first produce
the NWS-Char to exemplify the potential of appropriate technology for wood waste
utilization. The NWS-Char will then undergo surface morphology and elemental
composition to evaluate its characteristics. After which, NWS-Char will undergo
pyrolysis to fabricate the NWS-AC. The NWS-AC will be assessed through TGA for
its stable and efficient operational functionality and CV to evaluate its
electrochemical capacitance and whether it behaves like an ideal capacitor.

24
 CHAPTER 3
Materials and Methods

Figure 9. Schematic Diagram of the Methodology

25
Research Design

The activated carbon to be tested will be derived from NWS as a potential

electrode material. The product is expected to have a significant effect as an activated
carbon and differences with the commercially available materials in terms of surface
morphology, elemental composition, thermal resistivity, and electrochemical
performance. Thus, the product will undergo characterization—SEM and EDX—then
thermal and electrochemical analyses afterwards. Moreover, the study will be
performed with 4 set-ups with varying carbonization temperature to be compared with
one another before the testings for thermal resistivity and electrochemical properties
are carried out.

Phase 1 – Gathering of Materials

1 kg of NWS will be obtained from Ronniel Narra Furniture, 312C Roosevelt

Avenue, 1105 Quezon City. 300 mL of purified water and 50 mL of distilled water
will be bought from Mercury Drug Store. At the Air Zone Gas Trading at 200 A.
Bonifacio, N.S. Amoranto, Quezon City, 50 lbs of Nitrogen gas tank will be bought.
A 20 oz plastic bottle will be obtained at the Pasay City Public Market, Libertad
Street corner, Taft Avenue, Pasay City, Philippines. 100 mL of 37% Hydrochloric acid
(HCl) and 4 g of Sodium Nitrite will be purchased from Patagonian Enterprises, 1612
Remigio St, Sta. Cruz 121, Manila, 1003 Metro Manila. 100 g of desiccator silica gel,
1 L of deionized water, and 455 g of KOH will be acquired at Puljed Trading, 1336
Rizal Ave, Santa Cruz, Manila, 1003 Metro Manila. The CGA 580 Gas Regulator
with a female inlet and male outlet and a CGA 580 Nitrogen compressed gas flex
hose will be bought from ZIG3 Industrial Gas Trading Co. Ltd. at 191-E Tandang
Sora Ave. Quezon City.

26
Phase 2 – Production of Narra Wood Sawdust Activated Carbon (NWS-AC)

2.1 Carbonization of NWS

The NWS will be cleaned using purified water to remove impurities and dust.
Afterward, the sawdust will be dried overnight in a drying oven located at Adamson
University (ADU) Chemistry Laboratory at 110°C to reduce its moisture content.
Then, the NWS will be placed in a muffle furnace located at ADU Chemistry
Laboratory and heated up to 400°C at a heating rate of 6°C/min to produce the
NWS-Char. The NWS-Char will be kept at a specific temperature, and to achieve this,
it will be placed under a Nitrogen gas atmosphere for 1 hour at a pressure of 14.70 psi
(Aladin et al., 2021; Phainuphong et al., 2022). The Nitrogen gas tank will be
connected to the gas inlet of the muffle furnace via a CGA 580 Gas Regulator with a
female inlet and male outlet and a CGA 580 Nitrogen compressed gas flex hose
(CONCOA CGA Connection Reference Chart, n.d.; 1500oc Compact Muffle Furnace
(4.7"X4.7"X 4.7",1.7L) with 30 Segement Programmable Controller - KSL-1500X-S,
2024). The NWS-Char will then be kept in a desiccator silica gel to prevent moisture.

2.2 Impregnation Chemical Activation of the NWS-Char

Four 500 mL beakers will be labeled as Beaker A, Beaker B, Beaker C, and

Beaker D. Beaker A will contain 50 g of NWS-Char and 50 g of KOH to produce an
impregnation ratio of 1:1. Beakers B, C, and D will contain 50 g of NWS-Char and
150 g of KOH to produce an impregnation ratio of 1:3. Then, 300 mL of purified
water will be added to all four beakers to dissolve the chemical activating agent and
produce the KOH solution. After adding the water, Beakers A through D will be
stirred using a magnetic stirrer for 24 hours (Oladimeji et al., 2021; Phainuphong et
al., 2022). The processes mentioned above will take place in the PCNSciHS
laboratory.

27
 2.3 Production of NWS-AC with Varying Carbonization Temperatures

All the samples in this study will be labeled as Set-ups A through D. Set-ups
B, C, and D will have an impregnation ratio of 1:3, and the carbonization temperature
will be 700°C, 800°C, and 900°C respectively. Set-up A, which is the control group of
the study, will have an impregnation ratio of 1:1 and a carbonization temperature of
900°C. All Set-ups will then be heated using a muffle furnace located at ADU
Chemistry Laboratory with a heating rate of 6°C/min for 3 hours under a Nitrogen gas
atmosphere. Afterward, the NWS-AC samples will be cooled to room temperature
and immersed in 0.1 molar of HCl for 3 hours at ambient temperature before being
washed with deionized water to obtain a neutral pH. Subsequently, the NWS-AC
samples will be dried in a drying oven at ADU Chemistry Laboratory at 110°C for 12
hours and kept in a desiccator silica gel to prevent moisture (Oladimeji et al., 2021;
Phainuphong et al., 2022).

Phase 3 – Characterization and Testing

To determine the effectiveness of the activated carbon derived from the NWS
as an electrode material, characterization and testing must be done. Specifically,
Scanning Electron Microscope (SEM), Energy Dispersive X-ray (EDX),
Thermogravimetric Analysis (TGA), and Cyclic Voltammetry (CV);

3.1 Scanning Electron Microscope with Energy Dispersive X-Ray

(SEM/EDX)

The surface morphology of the NWS-char, its physical structure, and its
elemental analysis will be determined through SEM/EDX at the DLSU-Laguna
laboratory. Ogungbenro et al. (2018) stated that SEM is used to describe the physical
characteristics of chars, offering a visual representation of the raw material and chars
obtained at moderate and elevated pyrolysis temperatures. In addition, the analytical
data of SEM/EDX can be integrated with image processing and analysis
methodologies to furnish a statistical characterization of particles in relation to both
their chemical composition, morphology, and surface composition of the particles of

28
wood dust (Vandlíčková et al., 2020). SEM/EDX shall be conducted to assess its
suitability as an electrode material in terms of its elemental characteristics and
potential electrochemical performance.

3.2 Thermogravimetric Analysis (TGA)

TGA will be used to determine the thermal behavior of the NWS-AC. As

Abraham et al. (2018) stated, TGA measures the sample’s mass in relation to
temperature or time. In a study conducted by Nyombi et al. (2018), TGA was used to
study ash wood sawdust pyrolysis effectively, which allows researchers to control the
atmosphere and heating rate and ensures minimal temperature differences and mass
transport during the experiment. The test will be done at the ADMATEL of DOST.

3.3 Cyclic Voltammetry (CV)

In order to evaluate the electrochemical capacitance characteristic of the

NWS-AC, the CV test will be performed using the potentiostat. In addition, this test is
performed by cycling the potential of a working electrode and measuring the resulting
current (Libretexts, 2023), which can help identify the shape and position of the CV
and provide insight into the electrochemical activity of the NWS-AC. This will obtain
valuable information about electrode material's redox behavior, electrochemical
activity, and stability. This test will be done at ADU Chemistry Laboratory.

Collection of Data

The results to be obtained from the characterization and testings will undergo
One-Way ANOVA to statistically determine the differences between data obtained
and analyze the outcomes. This will shed light on the significant results evident on the
activated carbon derived from NWS as a potential material for electrodes.

29
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36
 APPENDIX A

Budget Report

Table 1. Budget of Materials

Description Quantity Unit Unit Cost (Php) Total Cost

(Php)

Narra sawdust 1 kg 0 0

Purified water 300 mL 10 10

Distilled water 50 mL 10 10

Nitrogen gas tank 50 lbs 800 800

Plastic bottle 1 pcs. 0 0

37% 100 mL 150 (per 100 mL) 150

Hydrochloric
Acid (HCl)

Desiccator silica 100 g 180 (per 100g) 180

gel

Deionized water 1 L 100 (per 1L) 100

Potassium 455 g 120 (per 50g) 1,200

Hydroxide
(KOH)

CGA 580 Gas 1 pc 6,500 6,500

Regulator with
hose

Muffle Furnace - - 800 (for the first 3,100

hour)
500 (per
succeeding hour)

37
 Description Quantity Unit Unit Cost (Php) Total Cost
(Php)

Drying Oven - - 500 (for the first 8,200

hour)
300 (per
succeeding hour)

Grand Total 20,250

1 kg of NWS will be obtained from Ronniel Narra Furniture, 312C Roosevelt

Avenue, 1105 Quezon City. 300 mL of purified water and 50 mL of distilled water
will be bought from Mercury Drug Store. At the Air Zone Gas Trading at 200 A.
Bonifacio, N.S. Amoranto, Quezon City, 50 lbs of Nitrogen gas tank will be bought.
A 20 oz plastic bottle will be obtained at the Pasay City Public Market, Libertad
Street corner, Taft Avenue, Pasay City, Philippines. 100 mL of 37% Hydrochloric acid
(HCl) and 4 g of Sodium Nitrite will be purchased from Patagonian Enterprises, 1612
Remigio St, Sta. Cruz 121, Manila, 1003 Metro Manila. 100 g of desiccator silica gel,
1 L of deionized water, and 455 g of Potassium Hydroxide (KOH) will be acquired at
Puljed Trading, 1336 Rizal Ave, Santa Cruz, Manila, 1003 Metro Manila. The CGA
580 Gas Regulator with a female inlet and male outlet and a CGA 580 Nitrogen
compressed gas flex hose will be bought from ZIG3 Industrial Gas Trading Co. Ltd.
at 191-E Tandang Sora Ave. Quezon City.

38
Table 2. Budget of Testings

Testings No. of Unit Cost (Php) Total Cost (Php)

Samples

Scanning Electron 1 1500/sample 1,500

Microscopy coupled
with Energy Dispersive
X-ray (SEM/EDX)

Thermogravimetric 4 2560/sample 10,240

Analysis (TGA)

Cyclic Voltammetry 4 - -
(CV)

Grand Total 11,740

Scanning Electron Microscopy with Energy Dispersive X-ray (SEM/EDX)

analysis will be conducted at De La Salle University-Laguna's laboratory
(DLSU-Laguna). Thermogravimetric Analysis (TGA) will be carried out at the
Advanced Device and Materials Testing Laboratory (ADMATEL) under the
Department of Science and Technology (DOST). Cyclic Voltammetry (CV) testing
will be conducted at Adamson University's Chemistry Laboratory (ADU).

Table 3. Budget of the Research Study

Budget Total Cost (Php)

Materials 20,250

Tests 11,740

Grand Total 31,990

39
APPENDIX B

Time Table

40
 APPENDIX C

Researchers’ Profile

Name Picture Address Birthday Contact

Number

Ana Maria B8 L1 January 22, anamedallaa@g

Rachel B. Avocado St., 2006 mail.com
Medalla Pasay City 17 years old

Rai Jeriele C. 218 E H. March 1, 2006 raipaliza030106

Paliza Domingo 17 years old @gmail.com
Street, Pasay
City

Nina Rhen 1857 September 9, jasminetorres09

Jasmine B. Cuyegkeng 2006 09@gmail.com
Torres Street, Pasay 17 years old
City

Vhera Maye 4 Gladiola November 18, vheramaye.umil

B. Umila Street, Pasay 2005 a@depedpasay.
City 18 years old ph

41