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RV College of
Engineering
Minor Project Presentation

Synthesis of Electrode materials for

Supercapacitors
Under the Guidance of:
Submitted by:
Vaishali Kharpuse             1RV20EE060
Dr. Ajay KM
Pragya Singh                    1RV20EE066
Assistant Professor
Vibhu Dixit                      1RV20EE070
Department of Electrical and Electronics
Rahul R                           1RV20EE073
RV College of Engineering

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Introduction Go, change the world

Energy Storage Devices

• Energy storage has evolved from Batteries

and fuel cells  Capacitors  Super

Super Capacitors
Capacitors Capacitors
• Shift towards sustainability

Batteries • Low supply current for memory backup in

and fuel
cells static random access memory(SRAM).
Sustainability

Fig. 1: Energy Storage Devices

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 RV College of
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• Performance of energy storage devices is analyzed

by Energy Density and Power Density
• Batteries and fuel cells: Greater Energy Densities
but Low Power Density
• Capacitors: Greater Power Densities but Lower
Energy Densities
• Super capacitors: Efficient trade-off between
Energy and Power Densities Fig. 2: Ragone Plot, Power density vs. Energy density
for various energy storage devices

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Fig. 3: Classification of Supercapacitors

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Engineering Introduction Go, change the world

Problem Statement

Conventional Super
Energy Storage Capacitors
Devices

High Energy and Po

To develop a Metal Chalcogenide nanomaterial
wer
densities
Specificity of Elect
rolyte through Green Synthesis method for super
to be used Cost effective mat
er ials

No fair balance be
power and energy
tween capacitor applications exploiting the advantages
density Easy synthesis of
materials

Degradation of elec
trodes Mitigates disadvan
and mitigating the disadvantages of conventional
tage
of other conventio s
nal
methods
energy storage devices, aiming at effective and

sustainable energy storage.

Fig. 4: Advantages of Supercapacitors

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Introduction Go, change the world

Objectives

• To synthesize Metal Chalcogenide nanomaterials using Green Synthesis method .

• Perform micro-structural Characterizations (XRD, SEM).

• To test the synthesized nanomaterials for its Electrochemical Properties i.e., Redox Properties, Specific

Capacitance, Power Density, Energy Density.

Future Objectives:-

• To develop Coin Cell using the nanomaterials that have been tested and yielded good Electrochemical

Results.

• Controlled discharge of the developed supercapacitor.

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Materials and Methodologies Go, change the world

Material Selection

Hydrothermal
Method Synthesis of Metal Chalcogenides

XRD – –Crystal
XRD Structures
Crystal Structures

Characterization of Metal Chalcogenides SEM – Surface Morphology

EDX – Surface Topography

Cyclicvoltammetry

Preparation of Electrode and Testing

Chronopotentiometry

Development of Supercapacitors

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 RV College of
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Theory and Concepts

Cyclic Voltammetry (CV)

• To investigate the Reduction and Oxidation Processes of
molecular species
• Top Curve: Reduction Curve; Bottom Curve: Oxidation
Curve
• Area under graph = Specific Capacitance
• The Scan Rate of the experiment controls how fast the applied
potential is scanned

Figure 5: Sample graph of CV test

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 RV College of
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Theory and Concepts

Chronopotentiometry (CP)
• To investigate the Charge and Discharge Properties of
molecular species
• Cycle: A repetitive loop of Charging and Discharging
• Specific Capacitance depends on Discharge Time
• The time of Charge and Discharge depends on Current
Density supplied to the material
Td: Discharge Time
i: Current
m: mass loading
∆:Potential Window

Figure 6: Sample graph of CP test

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Electrochemical Tests for Supercapacitors

Fig. 7: Cyclic Voltammetry (CV) Fig. 8: Electrochemical Setup Fig. 9: Chronopotentiometry (CP)
Common for both
CV and CP

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Materials and Methodologies Go, change the world

Chemicals Used and Compounds Synthesized

Table 1: Chemicals Used

Chemicals Used Molecular Formula

Nickel Nitrate Hexahydrate Ni(NO3)2 . 6H2O
Sodium Sulfide Na2S
Distilled Water H2O

Table 2: Compounds Synthesized

Compounds Synthesized Molecular Formula

Fig. 10: Nickel Sulfide

Fig. 11: Hydrothermal Method Nickel Sulfide NiS2

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Stoichiometric Calculations

Nickel Nitrate Sodium Sulphide 8 0 mL Water

290 g + 78 g +CTAB+ ¿ 100 mL → Nickel Sulphide
4.49 g 1.22 g Teflon Tube

CTAB:Cetrimonium bromide

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Materials and Methodologies Go, change the world

Hydrothermal Synthesis
Preparation of Solution
• Easiest method of Synthesis

Transfer solution to Autoclave under • Employs High Pressure and High Temperature
Hydrothermal Heating at 180°C for 2 hours • Result is a Suspension of particles

Cleaning and Centrifuging at 7000 rpm Green Synthesis:

• Distilled water is the medium of dissolution

Drying at 80°C for 2 hours • Ascorbic Acid (Vitamin C) used as Reducing Agent
• Non toxic chemicals used
• Sustainable temperature for Hydrothermal of 180°C
Metal Chalcogenide Nano Particles

Figure 12: Synthesis Methodology

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Characterizations and Facilities used

X-Ray Diffraction (XRD)

Scanning Electron Microscopy (SEM)
Electrochemical Analysis (CV, CP)

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Electrochemical Setup

3 Electrode System
• Working electrode – Material Coated onto Toray Carbon
• Counter electrode – Platinum Wire
• Reference electrode – Standard Calomel Electrode
• An Electrolyte – 2M Potassium Hydroxide solution
• CH Instruments Electrochemical Analyzer

Figure 13: Electrochemical Work Station

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Engineering Materials and Methodologies
Working Electrode Preparation
Electrode Preparation:
Sample PVDF NMP
• Weigh bare Electrode
• 80% of Sample + Carbon Black – 10% of weight of Bare Electrode

Sample
• 5% PVDF (Polyvinylidene Fluoride) binder
• 5% NMP (N-Methyl Pyrrolidone) binder
• Mix well using Mortar and Pestle Apply Sample onto
Aluminium Foil
• Apply onto Electrode using aluminium foil
• Dry at 80 ℃ for 2 hours. Dry in Hot Air Oven
• Weigh electrode after drying to calculate weight of loaded At 80C for 2 hours
Apply Sample onto
sample Electrode

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For Hydrothermal method

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RV College of
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Materials and Methodologies Go, change the world

For Solution Combustion

method

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Work Done is Chemistry Laboratory Go, change the world
Engineering

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RV College of
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Results and Discussions Go, change the world

X-Ray Diffraction (XRD) Of NiS2

Using Debye Scherrer's
Equation
D
Where
D, is the size of the particle
K, is the sherrer’s
constant(k=0.94)
)
ß, is the full width at half
maximum (FWHM) of the
diffraction peak

Figure 14: NiS2 graph

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RV College of
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Scanning Electron Microscopy (SEM)

Element Weight % Atomic %

SK 27.64 43.58
Ni K 72.36 56.42
Totals 100 100

Figure 16: EDX (NiS2)

Figure 15: SEM (NiS2)

Average Particle Size: 58nm
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RV College of
Engineering Results and Discussions Go, change the world

Electrochemical Results – NiS2

Table 3: CV Results

Scan Rate Specific

Retention (%)
(mV/s) Capacitance (F/g)

2 1559.10 100
10 1066.45 68.40
20 963.11 61.77
40 871.22 55.88
50 839.83 53.87
100 685.77 43.98

Figure 17: CV Results

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 RV College of
Engineering Results and Discussions Go, change the world

Screening
• A method to understand if the material is working or not
• Employs the Chronopotentiometry Technique
• Trial performed at a Current Density of 1A/g or 0.001A

Table 4: Electrochemical Screening data of Synthesized Compounds

Metal Chalcogenide Potential Window (V) Discharging Time(s) Specific Capacitance (F/g)
Nickel Sulfide 0.47 211.95 450.95

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RV College of
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Results and Discussions Go, change the world

Electrochemical Results – NiS2

Table 5: CP Results
Current Specific
Retention (%)
Density (A/g) Capacitance (F/g)

1 450.95 100
2 369.39 81.91
3 331.30 73.46
4 302.14 66.99
5 278.72 61.81
8 231.49 51.33
12 188.94 41.89
Figure 18: CP Results

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Future objectives Go, change the world

Fabrication of Coin Cell

Figure 20: Parts of Coin Cell

Figure 19: Arrangement of Coin Cell

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References Go, change the world
1. Waseem Raza, Faizan Ali, Nadeem Raza"Recent advancements in supercapacitor technology“.Doi= "10.1016/j.nanoen.2018.08.013"
2. Zaharaddeen S. Iro, C. Subramani* , S.S. Dash "A Brief Review on Electrode Material for Supercapacitor ". doi: 10.20964/2016.12.50
3. Nathalie Devillers, Samir Jemei, Marie, Marie-Ceceile Pera"Review of characterization methods for supercapacitor modelling". Doi:
2013.07.116/1652-77W/120/0876
4. Jiajun Jiu, Zuomin Dong, Tianxu Jin, LI Liu,"Recent Advance of Hybrid Energy Storage Systems for Electrified Vehicles". Doi:
10.1109/MESA.2018.8449191.
5. 5. Ajay K M, M N Dinesh, “Synthesis and characterization of Deccan hemp plant- based electrode material for supercapacitor
applications”. ICPN- 2019, ISBN: 15517616 0094243X, DOI: 10.1063/5.0009000
6. Ajay K M, M N Dinesh “Performance studies of Bamboo based Nano Activated carbon electrode material for supercapacitor applications”
[IConAMMA 2019].
7. K M Ajay, M N Dinesh “Influence of various Activated Carbon based Electrode Materials in the Performance of Supercapacitor’’. ISBN:
1757899X 17578981 DOI: 10.1088/1757-899X/310/1/012083
8. Ajay K M, Gaurav Mishal, Siddanna, Shivayogi. B. N, M. N. Dinesh, “Performance Studies of Biomass derived RHAC and MgO
Nanocomposite Electrode Material for Supercapacitor Applications”.  ICTSGS -2021, Japan Paper is published in ECS Transactions in March
2022.
9. C. Tan et al., “Recent Advances in Ultrathin Two-Dimensional Nanomaterials,” Chem.Rev., vol. 117, no. 9, pp. 6225–6331, 2017, doi:
10.1021/acs.chemrev.6b00558.
10. A. González, E. Goikolea, J. A. Barrena, and R. Mysyk, “Review on supercapacitors: Technologies and materials,” Renew. Sustain. Energy
Rev., vol.58, pp. 1189–1206, 2016, doi: 10.1016/j.rser.2015.12.249.
11. A. Venkadesh, S. Radhakrishnan, and J. Mathiyarasu, “Eco-friendly synthesis and morphology-dependent superior electrocatalytic
properties of CuS nanostructures,” Electrochim. Acta, vol. 246, pp. 544–552, 2017, doi: 10.1016/j.electacta.2017.06.077.
12. N. Elgrishi, K. J. Rountree, B. D. McCarthy, E. S. Rountree, T. T. Eisenhart, and J. L. Dempsey, “A Practical Beginner’s Guide to Cyclic
Voltammetry,” J. Chem. Educ., vol. 95, no. 2, pp. 197–206, 2018, doi: 10.1021/acs.jchemed.7b00361.
13. S. R. Sitaaraman et al., “Role of graphene in NiSe2/graphene composites - Synthesis and testing for electrochemical supercapacitors,” Diam.
Relat. Mater., vol. 108, p. 107983, 2020, doi: 10.1016/j.diamond.2020.107983.
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Thank you!

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