SYNTHESIS AND ANALYSIS OF SUPERCAPACITORS

A PROJECT REPORT

Submitted by

T ATHUL (RA2312008010004)

Under the guidance of

Dr. ROJI MARJORIE S.

(Associate Professor, Department of Electronics & Communication
Engineering)

in partial fulfilment for the award of the degree

of

MASTER OF TECHNOLOGY

in

VLSI DESIGN

DEPARTMENT OF ELECTRONICS AND COMMUNICATION

ENGINEERING

COLLEGE OF ENGINEERING AND TECHNOLOGY

(Deemed to be University u/s 3 of UGC Act, 1956)

SRM Nagar, Kattankulathur- 603203
Kancheepuram District
Nov - 2024
 BONAFIDE CERTIFICATE

This is to certify that this report, of the project work for 20ECP603L- Project Work
Phase-I named “SYNTHESIS AND ANALYSIS OF SUPERCAPACITORS”
submitted in partial fulfilment of the requirement for the award of degree, M-Tech in
VLSI Design, by T ATHUL, RA2312008010004, is the Bonafide project work of the
student, who carried out under my supervision. Certified further that, to the best of my
knowledge the work herein has not been submitted for the award of this or any other
degree, on an earlier occasion on this or any other candidate.

Signature of the Guide Signature of the Professor In-Charge

Dr. Roji Marjorie S Dr. Ramachandran B

Associate Professor Professor
Department of ECE Department of ECE
SRM Institute of Science and Technology SRM Institute of Science and Technology
Kattankulathur Kattankulathur

This project report is submitted for the project university examination held on
_________ November- 2024, at Department of ECE, SRMIST, Kattankulathur

Internal Examiner-I Internal Examiner-I

 ACKNOWLEDGEMENT

I express my gratitude towards, "The SRM Institute of Science and Technology" Department
of Electronics and Communication Engineering for providing an opportunity to work on this
project and gain profound knowledge on working and understanding the project

I wish to express my deep sense of gratitude and sincere thanks to our Head of Department
Dr. M. Sangeetha, and PG Coordinator Dr. B. Ramachandran, Professor for their
encouragement and motivations during the project work.

I would like to express my sincere thanks to the Project Co-Ordinator Dr. J. Manjula,
Associate Professor and Panel members Dr. Ravikumar, Professor of Practice, Dr. S. Roji
Marjorie, Associate Professor and Dr. M. Valarmathi, Assistant Professor for their time
and knowledge to the implementation of this project.

I am very grateful to my guide Dr. Roji Marjorie S, Department of Electronics and

Communication Engineering, who has guided me with inspiring dedication, untiring efforts,
and tremendous enthusiasm in making this project successful and presentable.

I extend my gratitude and heartfelt thanks to all the teaching and non-teaching staff of the
Electronics and Communications Department and to my parents and friends, who extended
their kind cooperation using valuable suggestions and timely help during the course of this
project work.

T ATHUL
(RA2312008010004)

3
 DECLARATION

I hereby declare the Project Work for 20ECP603L-Project Work-phase-I entitled

“STYNTHESIS AND ANALYSIS OF SUPERCAPACITORS” to be submitted for the
Degree in Master of Technology is my original work as individual and the dissertation has not
formed the basis for award of any Degree, Diploma, Associate ship or Fellowship of similar
other titles. It has not been submitted to any other University/Institution for the award of any
Degree/Diploma.

Place : Chennai T ATHUL

Date : RA2312008010004

4
 ABSTRACT

This study presents the synthesis and analysis of high-performance supercapacitors using a
composite of polyaniline (PANI) and Iron Cobalt Oxide (FeCo₂O₄) as electrode materials,
chosen for their complementary electrical properties. Polyaniline, a conductive polymer, is
known for its excellent electrical stability and high capacitance, while FeCo₂O₄, a
pseudocapacitive metal oxide, offers high theoretical capacitance and favourable redox
activity. By combining these materials, the supercapacitors developed in this work are expected
to demonstrate improved capacitance, energy density, and cycle stability, addressing
limitations found in conventional carbon-based electrodes.

The research involves multiple key objectives: selecting and forming optimal composite
materials for the anode and cathode, developing simulation models to predict electrical
behavior, and synthesizing the supercapacitor with a focus on balancing performance and
practicality. Electrical characterizations, including cyclic voltammetry (CV) and galvanostatic
charge-discharge (GCD) tests, are performed to evaluate the synthesized supercapacitor's
performance. Additionally, structural and electrical characterization of the electrode materials
are conducted to further validate their properties. The influence of various electrolytes, both
aqueous and non-aqueous, on the device performance is analysed, offering insights into the
electrical stability and efficiency of the supercapacitor under different conditions.

Before synthesis, modelling and simulations are carried out to assess key metrics such as
terminal potential, cell voltage, cell current, and temperature effects. These parameters are
graphically represented to aid in understanding the expected behavior of the composite
electrode materials in practical applications. The outcomes of this research could significantly
contribute to the advancement of supercapacitor technology, potentially providing efficient
energy storage solutions for renewable energy systems and portable electronics.

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 TABLE OF CONTENTS

BONAFIDE CERTIFICATE ............................................................................................................... 2

ACKNOWLEDGEMENT.................................................................................................................... 3

DECLARATION .................................................................................................................................. 4

ABSTRACT ........................................................................................................................................... 5

TABLE OF CONTENTS……………………………………………………………………….…….6
LIST OF FIGURES………………..……………………………………………………….................8
CHAPTER: 1......................................................................................................................................... 9

INTRODUCTION................................................................................................................................. 9

1.1 OVERVIEW:…………………………………………………………………………………..…10

1.2 PROBLEM STATEMENT AND OBJECTIVES …………...………………………………...11

1.3 METHODOLOGY: ...................................................................................................................... 11

CHAPTER: 2....................................................................................................................................... 13

LITERATURE SURVEY ................................................................................................................... 13

CHAPTER: 3....................................................................................................................................... 16

REVIEW OF EXISTING SUPERCAPACITOR MATERIAL AND THEIR LIMITATION….16

CHAPTER: 4…………………………………………...…………………………………………….19

PROPERTIES, SYNERGISTIC BEHAVIOR, AND SYNTHESIS OF POLYANILINE AND

IRON COBALT OXIDE IN SUPERCAPACITORS……………………………………………....19

CHAPTER: 5…………………………………………………………………………………………23

RESULTS ............................................................................................................................................ 23

6.1 OBSERVATION:……………………………………………………………………...................26

6.2 ANALYSIS……………………………………………………………………………………….27

CHAPTER: 7....................................................................................................................................... 29

CONCLUSION AND FUTURE SCOPE .......................................................................................... 29

CHAPTER: 8....................................................................................................................................... 31

REFERENCE……………………………………………………………………………..………….31

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 LIST OF FIGURES

FIGURE 1: Block Diagram of Synthesis Process...……………………………………….…………..17

FIGURE 2: Pack Summary (Proposed vs Lithium Supercapacitor Model)…………………………..25

FIGURE 3: Cell Current (Proposed vs Lithium Supercapacitor Model)……………………………...25

FIGURE 4: Cell Internal Resistance (Proposed vs Lithium Supercapacitor Model)…………………25

FIGURE 5: Surface Open Circuit Voltage (Proposed vs Lithium Supercapacitor Model)…………..26

FIGURE 6: Terminal Voltage (Proposed vs Lithium Supercapacitor Model)………………………..26

FIGURE 7: Te,perature Curve of Proposed Supercapacitor Model ……...…………………………..26

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8
 CHAPTER: 1
INTRODUCTION

9
1.1 OVERVIEW:
Supercapacitors have emerged as promising energy storage devices, bridging the gap between
traditional capacitors and batteries by offering rapid charge-discharge cycles, high power
density, and long cycle life. Unlike batteries, which rely on faradaic reactions, supercapacitors
store energy primarily through electrostatic charge separation, leading to a faster response time
and enhanced durability. However, to meet the increasing demand for higher energy density in
renewable energy applications, electric vehicles, and portable electronics, innovative material
solutions are required to enhance the performance of supercapacitors.

This project focuses on the synthesis and analysis of supercapacitors using polyaniline (PANI)
and Iron Cobalt Oxide (FeCo₂O₄) as electrode materials. Polyaniline, a highly conductive
polymer, offers excellent electrical stability, significant capacitance, and favourable
conductivity, making it a strong candidate for enhancing supercapacitor performance. In
parallel, Iron Cobalt Oxide (FeCo₂O₄) is a pseudocapacitive material known for its high
theoretical capacitance, remarkable redox activity, and substantial contribution to energy
density. The combination of PANI and FeCo₂O₄ leverages the strengths of both materials,
aiming to achieve supercapacitors with superior capacitance, energy density, and long-term
stability, potentially outperforming traditional carbon-based supercapacitors.

Key objectives of this work include the selection of appropriate composite materials for the
anode and cathode, simulation and modelling of electrical behaviours, and synthesis of the
supercapacitor with a balance of high performance and ease of preparation. Structural and
electrical characterization is conducted to validate the properties of the synthesized electrode
materials. Electrical analyses such as cyclic voltammetry (CV) and galvanostatic charge-
discharge (GCD) tests are employed to measure the specific capacitance, energy density, and
cycle stability of the device. Furthermore, the supercapacitor's performance under various
electrolyte conditions—both aqueous and non-aqueous—is evaluated to understand the effects
of electrolyte composition on device efficiency and stability. Before synthesis, simulation
models provide insights into critical metrics such as terminal potential, cell voltage, cell
current, and device temperature. These parameters are visualized through plotted graphs,
offering a detailed understanding of the expected behaviour and performance of the composite
materials prior to synthesis. The findings from this study aim to contribute to the development
of next-generation supercapacitors with enhanced capabilities, aligning with the growing
global need for efficient and sustainable energy storage solutions.

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1.2 PROBLEM STATEMENT AND OBJECTIVES:
1. To select appropriate materials for both anode and cathode to form composite materials
with optimal properties for supercapacitor applications

2. To develop models for the selected electrode materials to simulate and analyse
electrical behaviours, including key metrics like terminal potential, cell voltage, and
cell current etc.

3. To synthesize the supercapacitor using a method that balances ease of preparation with
high performance.

4. To conduct structural and electrical characterization of the synthesized electrode

materials. Analyse the performance of the supercapacitor under the influence of
different electrolytes, including both aqueous and non-aqueous options.

1.3 METHODOLOGY:
This project investigates the electrical performance of a supercapacitor with polyaniline
(PANI) as the cathode and Iron Cobalt Oxide (FeCoOₓ) as the anode using the open-source
modelling framework PyBaMM. The research is structured into two phases: 1) simulation of
supercapacitor behaviour and 2) synthesis and experimental validation of material properties
and device performance. Here, we present the methodology for Phase 1, detailing the steps
taken to model, simulate, and analyse the charge/discharge behaviour of the supercapacitor.
To begin, a custom supercapacitor model was developed using PyBaMM to simulate the unique
electrical processes occurring in the PANI-FeCoOₓ electrode system. Each electrode was
modelled to capture its specific behaviour and properties. The pseudocapacitive behaviour of
PANI was represented by incorporating specific capacitance and characteristic
charge/discharge profiles, which simulate the double-layer and pseudo capacitance effects that
enable PANI to store charge. For FeCoOₓ, Faradaic reactions were included to reflect its redox
activity, critical to the anode’s charge/discharge processes. Potassium hydroxide (KOH) was
chosen as the electrolyte for its ionic conductivity and compatibility with the electrodes, with
the model capturing ion transport and interactions at the electrode-electrolyte interface.
Governing equations, including the Nernst-Planck equations and Butler-Volmer kinetics, were
used to simulate ion diffusion, charge transport, and the reaction kinetics at electrode

11
surfaces—particularly essential for the Faradaic charge storage in FeCoOₓ.
The supercapacitor model configuration featured a two-electrode setup with PANI as the
cathode and FeCoOₓ as the anode. This arrangement was designed to account for double-layer
capacitance and pseudocapacitive effects in PANI, along with Faradaic reactions in FeCoOₓ.
The Nernst-Planck equations enabled accurate representation of ion transport and
concentration gradients, while Poisson’s Equation and porous electrode theory enhanced the
simulation of electrostatic potential and ion diffusion within the porous electrode materials.
Simulating charge/discharge profiles involved setting up the model under constant current or
constant voltage conditions, with voltage limits and current rates defined to mimic real-world
operations. The simulation duration was set to capture both transient and steady-state
performance. Using PyBaMM’s solver (such as CasadiSolver), the simulation provided time-
dependent results, including voltage, current, and energy metrics across each cycle. Key
metrics, including terminal voltage, cell current, voltage drop during discharge, and recovery
characteristics between cycles, were tracked for analysis.
Data visualization involved referencing the Doyle-Fuller-Newman (DFN) model to graphically
represent ion concentration, potential, and ion transport within the electrolyte and electrodes.
Graphs were generated to capture electrode and electrolyte phase dynamics, and solid-phase
ion diffusion, to understand the material behaviour and charge storage characteristics better.
Important metrics such as terminal voltage, cell voltage, cell current, and temperature over time
were plotted to provide a detailed view of the anticipated supercapacitor performance before
synthesis.
The simulation findings give a foundational understanding of the supercapacitor's behaviour,
setting the stage for Phase 2 of the project, which will focus on material synthesis and
experimental validation. The chosen configuration of PANI and FeCoOₓ electrodes with a
KOH electrolyte shows promise as a high-performance supercapacitor, expected to enhance
energy density, capacitance, and cycle stability. These advancements align with the project's
broader goal of developing efficient, high-capacity energy storage solutions for applications in
renewable energy systems and portable electronics.

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 CHAPTER: 2
Literature Survey

13
2.1
Inal, I. I. G., Gokce, Y., & Aktas, Z. (2016). “Waste tea derived activated
carbon/polyaniline composites as supercapacitor electrodes.” In 2016 IEEE
International Conference on Renewable Energy Research and Applications
(ICRERA), Birmingham, UK (pp. 458-462). IEEE.
The study explores the development of activated carbon/polyaniline composites
derived from waste tea for supercapacitor electrodes, aiming to leverage the high
surface area and conductivity of the composite to enhance energy storage
capabilities.

2.2
Tarek, Y. A., et al. (2020). “One-Step Gel Formation Method for the
Synthesis of NiO-MnXOY Mixed Oxide Nanomaterials as a Prospective
Supercapacitor Material.” In 2020 2nd International Conference on
Sustainable Technologies for Industry 4.0 (STI), Dhaka, Bangladesh. IEEE.
This research presents a one-step gel formation method for synthesizing NiO-
MnXOY mixed oxide nanomaterials, demonstrating its potential for use in
supercapacitors due to its high capacitance and structural stability.

2.3
Raghav, J., & Roy, S. (2023). “Electrochemical Properties of Ternary Metal
Oxides for Supercapacitor.” In 2023 International Workshop on Impedance
Spectroscopy (IWIS), Chemnitz, Germany (pp. 67-72). IEEE.
The objective of this work is to examine the electrical properties of ternary metal
oxides as electrode materials for supercapacitors, focusing on improving specific
capacitance and enhancing stability under cycling conditions.

2.4
Yuan, M., Yu, J., & Chen, X. (2022). “Polyaniline Modified Laser-Scribed
Graphene for High-Performance Microsupercapacitors.” In IEEE Electron
Device Letters, 43(6), 966-969.
The paper investigates a microsupercapacitor design using polyaniline-modified
laser-scribed graphene, achieving enhanced energy density and charge-discharge
efficiency suitable for miniaturized energy storage applications.

2.5
Song, B., Moon, K.-S., & Wong, C.-P. (2016). “Recent Developments in

14
Design and Fabrication of Graphene-Based Interdigital Micro-
Supercapacitors for Miniaturized Energy Storage Devices.” In IEEE
Transactions on Components, Packaging and Manufacturing Technology,
6(12), 1752-1765.
This paper reviews recent advances in the design and fabrication of graphene-
based interdigital micro-supercapacitors, emphasizing improvements in energy
density, power output, and device miniaturization to meet the demands of
compact energy storage solutions.

2.6
Wang, X., Zhao, Q., & Tang, Y. (2021). “Synthesis of PANI/Graphene Composite for
High-Performance Supercapacitors.” In 2021 IEEE International Conference on Power
Electronics and Renewable Energy (CPERE), Shanghai, China (pp. 245-250). IEEE.
This study investigates the synthesis of polyaniline (PANI) and graphene composites as
supercapacitor electrodes. The goal is to combine the pseudocapacitive behavior of PANI with
the high conductivity of graphene to achieve enhanced energy density, capacitance, and cycle
life for energy storage applications.

2.7
Kim, H., Lee, J., & Park, S. (2019). “Enhanced Capacitance in FeCoOₓ-Based
Supercapacitors Using KOH Electrolyte.” In IEEE Transactions on Energy Conversion,
34(5), 1073-1080.
The objective of this paper is to improve the electrical performance of FeCoOₓ-based
supercapacitors by employing KOH as the electrolyte. The study highlights the increased
capacitance and stability achievable through optimizing electrolyte concentration and electrode
synthesis techniques, providing insights relevant to high-efficiency supercapacitor designs.

15
 CHAPTER: 3
Review of Existing Supercapacitor
Materials and Their Limitations

16
In recent years, supercapacitors have gained considerable attention as a solution for energy
storage applications due to their high power density, rapid charge/discharge capabilities, and
extended cycle life. A significant area of research within this field has focused on developing
materials that enhance these properties, with various designs and composites tested to
maximize the energy density, stability, and overall performance of supercapacitors. Despite the
advances, each material category presents limitations that hinder optimal performance,
emphasizing the need for innovative material solutions. This chapter reviews widely researched
supercapacitor materials, examining their benefits and limitations to provide context for the
subsequent focus on polyaniline (PANI) and iron cobalt oxide (FeCoOₓ) as promising
alternatives.

Carbon-based materials, including activated carbon, carbon nanotubes, and graphene, have
been widely used as supercapacitor electrodes due to their high surface area, electrical
conductivity, and relatively low cost. Activated carbon, in particular, is well-known for its high
porosity, which facilitates double-layer capacitance and enables rapid charge/discharge cycles.
However, carbon-based materials generally suffer from lower energy density compared to
pseudocapacitive materials, limiting their applicability in high-energy-demand applications.
Research by Inal et al. (2016) attempted to improve this limitation by combining activated
carbon with polyaniline, creating composites that offer both high capacitance and better
conductivity. Despite such advancements, carbon-based materials typically lack the redox
activity needed for substantial energy density, thus requiring further enhancement or pairing
with pseudocapacitive materials.

Metal oxides, such as manganese oxide (MnO₂), nickel oxide (NiO), and cobalt oxide (Co₃O₄),
exhibit pseudocapacitance due to their ability to store energy through Faradaic reactions. These
materials offer higher energy densities than purely carbon-based electrodes; however, they face
challenges related to structural stability and cycling degradation. Mixed oxides, such as NiO-
MnXOY, synthesized using advanced methods like the one-step gel formation method reported
by Tarek et al. (2020), have demonstrated improved stability and capacity retention. Despite
these improvements, the performance of metal oxides can still suffer due to their relatively low
electrical conductivity and susceptibility to structural changes during repetitive
charge/discharge cycles. These limitations highlight the need for materials that can retain
structural integrity and enhance cycle life without sacrificing electrical performance.

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Conductive polymers like polyaniline (PANI) and polypyrrole (PPy) have gained interest as
supercapacitor materials due to their pseudocapacitive behavior, high conductivity, and ability
to support rapid charge storage. PANI, for instance, is well-regarded for its high theoretical
capacitance and relatively low synthesis cost, making it an attractive choice for energy storage
devices. However, conductive polymers often suffer from poor cycle stability, with significant
degradation in capacitance observed over repeated charge/discharge cycles due to the
polymer’s swelling and contraction. As a result, researchers have focused on developing
composites that combine conductive polymers with other materials to improve cycle life and
mechanical durability. Yuan et al. (2022) demonstrated one approach to addressing these
limitations by modifying laser-scribed graphene with PANI, thereby enhancing charge-
discharge efficiency in microsupercapacitor applications. Nonetheless, achieving long-term
stability remains a challenge with conductive polymers, particularly in applications requiring
high cycle counts.

Recent studies have also explored transition metal compounds, such as FeCoOₓ, and hybrid
materials, which incorporate properties of both carbon-based and pseudocapacitive materials.
These compounds show promise due to their high theoretical capacitance, electrical stability,
and ability to facilitate efficient charge transfer through redox reactions. Research by Kim et
al. (2019) on FeCoOₓ, for example, indicated that using KOH as the electrolyte could improve
the material’s pseudocapacitive behavior and overall performance. However, challenges
remain in optimizing the synthesis processes and balancing the trade-offs between high
capacitance and structural stability under cycling conditions. Hybrid materials have attempted
to bridge these gaps by combining conductive polymers or carbon-based materials with metal
oxides, aiming to leverage the strengths of each component. However, achieving a scalable and
cost-effective synthesis process remains a significant obstacle.

Despite progress in supercapacitor material design, significant limitations persist across

different material types. Carbon-based materials, though conductive and cost-effective,
struggle to achieve high energy density. Metal oxides and mixed oxides exhibit better
capacitance but face issues related to conductivity and stability. Conductive polymers offer
high capacitance but are prone to cycle degradation, while hybrid materials present promising
performance metrics yet often involve complex and costly synthesis methods. These limitations
drive the ongoing search for materials that can deliver high energy density, stability, and
affordability in a single configuration. The next chapter will build upon these studies by
focusing specifically on the potential of PANI and FeCoOₓ as electrode materials.

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 CHAPTER: 4
Properties, Synergistic Behavior,
and Synthesis of Polyaniline and
Iron Cobalt Oxide in
Supercapacitors

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Polyaniline (PANI) and Iron Cobalt Oxide (FeCo₂O₄) are promising materials in the field of
supercapacitor research due to their unique electrical properties and complementary
functionalities. Individually, both materials offer characteristics valuable for energy storage
applications, and when combined, they form a composite that significantly enhances the
performance of supercapacitors. This chapter explores the properties of PANI and FeCo₂O₄,
their roles as electrode materials, the synergistic benefits of their combination, and the synthesis
methods employed to produce this composite.

Polyaniline, a conductive polymer, is known for its excellent electrical conductivity,

environmental stability, and ease of synthesis. A notable characteristic of PANI is its tunable
conductivity, which can be adjusted through doping and structural modifications to improve its
electrical performance. This adaptability allows PANI to exhibit high specific capacitance,
rapid charge/discharge rates, and stable, reversible redox reactions. These reactions enable
PANI to efficiently store and release charge, making it ideal for supercapacitors that require
fast energy delivery and recovery. PANI’s high specific capacitance and reversible redox
behavior also contribute to higher power density and reliability, which are essential for high-
performance energy storage systems. Its stability in various environmental conditions further
enhances the durability and longevity of supercapacitors that utilize it.

Iron Cobalt Oxide (FeCo₂O₄), a ternary metal oxide, complements PANI with its high electrical
conductivity, allowing rapid charge transport, especially under high-demand conditions.
Formed from both iron and cobalt, FeCo₂O₄ combines the stability of iron oxides with the redox
activity of cobalt, resulting in superior electrical properties and stability. FeCo₂O₄’s porous
structure and large surface area provide ample active sites for electrical reactions, which boosts
the material’s charge storage capacity. The high surface area and redox activity of FeCo₂O₄
enable it to reach high capacitance values and support efficient charge/discharge cycles. Its
stability in both aqueous and non-aqueous electrolytes ensures adaptability for various
supercapacitor configurations, enhancing its durability across diverse operating conditions.

When combined, PANI and FeCo₂O₄ create a composite material that capitalizes on each
component’s strengths, leading to enhanced energy density, capacitance, and cyclic stability in
supercapacitors. PANI’s high conductivity ensures efficient electron transfer, while FeCo₂O₄’s
pseudocapacitance significantly boosts charge storage capacity through Faradaic reactions.
This synergistic effect greatly enhances the overall capacitance and energy storage capabilities

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of the supercapacitor. By integrating PANI’s conductivity and stability with FeCo₂O₄’s redox
activity and structural robustness, the composite achieves a superior balance of power and
energy density. This enhancement is particularly beneficial for applications requiring rapid
charge/discharge cycles, such as portable electronics and renewable energy storage.
The PANI-FeCo₂O₄ composite offers not only improved energy storage but also enhanced
cyclic stability, which is critical for long-term supercapacitor applications. FeCo₂O₄’s high
porosity accommodates the volume changes during charge/discharge cycles, while PANI’s
flexibility stabilizes the structure, preventing degradation over time. The redox activities of
both FeCo₂O₄ and PANI support consistent charge storage and release, contributing to
increased energy and power density. Additionally, the electrolyte selection significantly
impacts the composite’s performance. Aqueous electrolytes, such as KOH, provide high ionic
conductivity and facilitate efficient ion transport, which is essential for high power output.
Conversely, non-aqueous electrolytes offer a broader electrical stability window, allowing
higher operational voltages and, consequently, greater energy storage.
Synthesis Methods for PANI-FeCo₂O₄ Composite
The synthesis of the PANI-FeCo₂O₄ composite is a crucial step to ensure optimal electrical
properties for supercapacitor applications. Several synthesis techniques can be employed to
achieve a uniform composite structure with enhanced electrical conductivity and capacitance.
The following methods are commonly used:
1. In Situ Polymerization: This method involves the polymerization of aniline in the
presence of FeCo₂O₄ nanoparticles. The FeCo₂O₄ particles are dispersed in an aniline
solution, and a polymerizing agent (e.g., ammonium persulfate) is added to initiate the
formation of PANI. This method allows for a uniform distribution of FeCo₂O₄ particles
within the PANI matrix, resulting in enhanced electron conductivity and redox
behavior.
2. Hydrothermal Synthesis: In this approach, FeCo₂O₄ is synthesized in a hydrothermal
reactor using cobalt and iron precursors. The process involves heating an aqueous
solution of metal precursors at high temperatures under pressure, resulting in the
formation of FeCo₂O₄ nanoparticles with high crystallinity. Once formed, the FeCo₂O₄
particles are combined with PANI using either in situ polymerization or simple physical
mixing.
3. Electrochemical Deposition: This technique involves applying an electric field to
deposit PANI onto a substrate containing FeCo₂O₄ particles. The electric field drives

21
 the polymerization of aniline monomers, creating a thin layer of PANI on the FeCo₂O₄
particles. Electrical deposition can produce a highly uniform composite structure and is
particularly suitable for applications requiring thin-film supercapacitors.
4. Physical Mixing and Compression: In this method, PANI powder and FeCo₂O₄
nanoparticles are physically mixed, followed by compression or pelletization to form a
compact electrode material. Although simpler, this technique may result in less uniform
dispersion of FeCo₂O₄ within the PANI matrix and may not achieve the same level of
performance as the in situ or electrical methods.
The selected synthesis method significantly influences the electrical properties of the resulting
PANI-FeCo₂O₄ composite. For instance, in situ polymerization and electrical deposition
generally yield composites with higher surface area, uniform particle dispersion, and better
electrical conductivity. These synthesis methods enhance the synergistic effects of PANI and
FeCo₂O₄, contributing to greater capacitance, energy density, and cycle stability in
supercapacitor applications.

Figure 5: Block Diagram of Synthesis Process)

22
CHAPTER: 5
Results

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 Figure 2: Pack Summary (Proposed vs Lithium Supercapacitor Model)

Figure 3: Cell Current (Proposed vs Lithium Supercapacitor Model)

Figure 4: Cell Internal Resistance (Proposed vs Lithium Supercapacitor Model)

24
Figure 5: SOC Voltage (Proposed vs Lithium Supercapacitor Model)

Figure 6: Terminal Voltage (Proposed vs Lithium Supercapacitor Model)

Figure 7: Temperature Curve of Proposed Supercapacitor

25
5.1 Observations:
The proposed supercapacitor model demonstrates a higher steady-state voltage (Figure 2),
reaching a peak of 4.1V before stabilizing at 4.0V after 12,000 seconds of charging. This
indicates a higher energy storage capacity compared to the lithium-based model, which peaks
at 4.1V but stabilizes at 3.8V within 6,000 seconds. Both models eventually stabilize at a
current of zero, suggesting efficient charge retention. The proposed model’s ability to achieve
a higher steady-state voltage highlights its potential for greater energy storage.

The proposed model shows a high initial current (Figure 3) that rapidly decreases to nearly 0V,
indicating a faster stabilization. In contrast, the lithium-based supercapacitor begins with a
lower initial current but stabilizes at a higher current value. This difference in current behavior
reflects the distinct charge/discharge kinetics of the two models, with the proposed model
exhibiting quicker energy stabilization.

The peak internal resistance (Figure 4) for the proposed supercapacitor model is observed to
be 0.034 ohms, slightly higher than the 0.028 ohms observed in the lithium-based model. While
both models demonstrate relatively low internal resistance, this difference suggests that the
proposed model might experience slightly higher internal losses during charge/discharge
cycles, which could impact overall efficiency.

For the proposed supercapacitor, the surface open-circuit voltage (Figure 5) starts at 4.2V,
drops to 3.5V, and then increases back to 4.0V over a 12,000-second period. In comparison,
the lithium-based supercapacitor exhibits a different voltage pattern, fluctuating between
3.75V, 4.1V, and 3.8V within a 6,000-second span. The observed voltage fluctuations in the
proposed model indicate dynamic behavior and energy storage changes over time, which can
inform its stability and charge retention performance.

The terminal voltage (Figure 6) of the proposed model shows a drop from 4.05V to 3.4V and
then recovers to 4.0V over 12,000 seconds. This variation in terminal voltage suggests an
adaptive charge/discharge cycle, characteristic of supercapacitors, where the voltage initially
drops before stabilizing. In contrast, the lithium model may demonstrate a smoother voltage
stabilization but with a lower final voltage value, which is indicative of differences in
charge/discharge efficiency between the two materials.

26
The proposed supercapacitor operates effectively in the temperature range (Figure 7) of 300K
to 330K (26.85°C to 56.85°C), suggesting that it can function under moderate to higher
temperatures without significant performance degradation. This temperature range is crucial
for real-world applications where temperature fluctuations are common, and the ability of the
supercapacitor to maintain stable performance in such conditions enhances its practicality.

5.2 Analysis

The comparative analysis of the proposed supercapacitor model, utilizing PANI as the cathode
and iron cobalt oxide (FeCoOₓ) as the anode, reveals several advantages and unique
characteristics over the lithium-based supercapacitor model.

Starting with the steady-state voltage characteristics (Figure 2), the proposed model reaches a
peak voltage of 4.1V and stabilizes at 4.0V after 12,000 seconds of charging. This is a notable
improvement over the lithium-based model, which, despite peaking at the same voltage,
stabilizes at a lower value of 3.8V within a shorter 6,000-second span. This extended
stabilization period and higher steady-state voltage suggest a greater energy storage capacity,
which is beneficial for applications requiring sustained power output. Both models, however,
eventually stabilize at a zero-current state, indicating efficient charge retention.

The initial current behavior (Figure 3) further highlights the advantages of the proposed model.
It exhibits a high starting current, which quickly declines to nearly zero, reflecting rapid
stabilization and efficient charging kinetics. In contrast, the lithium-based model starts with a
lower initial current and stabilizes at a relatively higher current, suggesting different
charge/discharge dynamics. The proposed model's quicker stabilization could lead to more
efficient energy storage and retrieval, which is valuable for applications requiring rapid energy
access.

Examining internal resistance (Figure 4), the proposed supercapacitor demonstrates a peak
resistance of 0.034 ohms, slightly higher than the 0.028 ohms observed in the lithium-based
model. While both resistance values remain low, suggesting efficient energy transfer, the
marginally higher resistance in the proposed model may indicate a slight increase in internal
losses. This small difference could impact overall efficiency, although the proposed model's
advantages in energy storage and rapid stabilization may offset this minor drawback.

27
The surface open-circuit voltage behaviour (Figure 5) of the proposed model presents
interesting dynamics. Starting at 4.2V, the voltage drops to 3.5V and gradually increases back
to 4.0V over a period of 12,000 seconds. In comparison, the lithium-based supercapacitor
follows a different pattern, fluctuating between 3.75V, 4.1V, and 3.8V within just 6,000
seconds. These fluctuations in the proposed model reflect a dynamic energy storage process
and underscore its capability to adaptively retain charge over extended periods, enhancing
stability and reliability.

The terminal voltage behaviour (Figure 6) further supports these findings, as the proposed
model displays an initial drop from 4.05V to 3.4V before returning to 4.0V over the 12,000-
second duration. This adaptive cycle highlights the supercapacitor's characteristic
charge/discharge profile, where an initial voltage drop is followed by stabilization. In contrast,
the lithium-based model may show a smoother voltage transition but stabilizes at a lower final
voltage, suggesting that the proposed model can achieve higher charge/discharge efficiency,
advantageous for prolonged energy storage.

Lastly, the temperature resilience of the proposed supercapacitor (Figure 7) is noteworthy.

Operating effectively within a range of 300K to 330K (26.85°C to 56.85°C), the model
demonstrates stability across moderate to high temperatures, crucial for real-world applications
where thermal fluctuations are common. This stability in varying temperatures highlights the
practical utility of the PANI and FeCoOₓ-based supercapacitor, as it can maintain performance
without degradation across diverse environmental conditions.

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 CHAPTER: 6
Conclusion and Future Scope

29
In conclusion, the proposed supercapacitor model incorporating Polyaniline (PANI) as the
cathode and Iron Cobalt Oxide (FeCo₂O₄) as the anode demonstrates promising characteristics
for high energy storage and efficient charge/discharge behavior. The model exhibits higher
steady-state voltage and superior energy storage capacity compared to conventional lithium-
based models, with the ability to maintain stable performance across a range of temperatures.
The observed internal resistance and voltage fluctuations suggest that while the proposed
model offers enhanced performance, there may be areas for further optimization, particularly
in minimizing internal losses during charge/discharge cycles.

The observed differences in the behavior of the proposed supercapacitor, such as the rapid
stabilization of current and voltage, highlight the potential advantages of combining PANI and
FeCo₂O₄, leveraging the unique properties of both materials. This synergy not only improves
the overall energy density but also contributes to faster charge and discharge rates, which are
critical for practical applications in energy storage systems, including renewable energy storage
and portable electronics.

In terms of future scope, further investigation into the optimization of the synthesis process
will be crucial for enhancing the properties of the composite material. Future work will involve
experimenting with different synthesis conditions, such as adjusting precursor concentrations,
synthesis temperatures, and reaction times, to optimize the morphology, surface area, and
electrical conductivity of both PANI and FeCo₂O₄. By fine-tuning these parameters, it will be
possible to improve the material’s electrical performance, which is key to achieving better
energy storage and overall efficiency. Additionally, future studies will explore the impact of
various electrolytes—both aqueous and non-aqueous—on the supercapacitor’s performance,
with the goal of improving charge/discharge rates, stability, and lifespan.
The synthesis method will play a crucial role in better characterizing the supercapacitor’s
properties. Through the development and optimization of more advanced synthesis techniques,
it will be possible to control the microstructure and porosity of the composite material,
enhancing its energy storage capabilities. Further electrical characterization using techniques
such as cyclic voltammetry, impedance spectroscopy, and charge/discharge testing will provide
deeper insights into the supercapacitor’s performance, aiding in the refinement of its design for
specific applications. This continued research will help to optimize the performance of the
PANI-FeCo₂O₄ supercapacitor, advancing it toward real-world energy storage applications.

30
CHAPTER: 7
Reference

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