STATE OF THE ART

SEMINAR ON

SYNTHESIS OF ASYMMETRIC SUPERCAPACITOR ELECTRODES

WITH ENHANCED ELECTROCHEMICAL PROPERTIES

Supervisor: Dr. Bhawna Verma

Saurabh Kumar Pandey
PhD 3rd year
Department of Chemical
Engineering & Technology
Roll No-19041019
Contents
 Introduction of supercapacitors
 Ragone Plots for Energy Devices
 Characteristics and classification
 Applications, Advantages and Disadvantages
 Nanocomposite
 Conducting polymer
 Activated carbon
 Asymmetric supercapacitors
 Literature survey
 Research gap
 Working Plan
 List of Characterization Techniques
 Introduction
 Supercapacitors have drawn intensive attention owning to their virtues of high power
density, long life-cycle, short charging time and safe operation for promising applications.

 Supercapacitors are designed to bridge the gap between batteries and capacitors to form
fast-charging energy-storage devices of intermediate specific energy density.

 Supercapacitors are important devices in energy-storage and conversion systems and are
used in electric vehicles, uninterruptible power supplies (UPS) as well as in memory
protection of computer electronics and cellular devices.

 A supercapacitor differs from a conventional capacitor in that it has a very high

capacitance (in farads as compared to pico-microfarad range).

 Compared with lithium-ion batteries, supercapacitors also exhibit higher specific power
density.

 Supercapacitors mainly store electrical charge only at the electrode surface rather than
within the entire electrode, so that they tend to have lower energy densities as compared
to batteries.
 Conventional capacitor

 Capacitance C is defined as the

ratio of stored (positive) charge
Q to the applied voltage V

 For a conventional capacitor, C

is directly proportional to the
surface area A of electrodes and
inversely proportional to the
distance D between the
electrodes

Fig 1: Conventional capacitor

(schematic)
 Supercapacitor
Supercapacitors are governed by the same basic

principles as conventional capacitors

They incorporate electrodes with much higher surface

areas and much thinner dielectrics that decrease the

distance D between the electrodes

The conductivity through the separator is proportional

to its porosity (40–70%) and is represented by:

where is the electrolyte conductance, p is the

porosity and α is a power factor with 1.5<α<2.

Ragone plot of Energy devices

Fig 3: Ragone plot of various energy

devices
EDLC and Pseudocapacitance
Fig 4:
Schematic
representation
of EDLC
capacitor in its
charged state

Fig 5: Charge storage mechanism of pseudocapacitive

 Characteristics and classification of supercapacitors types

Type Electrode Operation Mechanism Properties

Electrostatic Carbon and carbon Electrochemical Double layer mechanism Good specific capacitance, Higher
(EDLC) derivatives power density, Long life, Higher
cyclic stability. Lower energy
density.

Pseudo Metal oxides, Conducting Reversible Faradaic reactions Higher specific capacitance, Higher
capacitor polymers energy density, Lower cyclic
stability

Hybrid capacitor

Asymmetric type Different electrode Combination of Reversible Faradaic Higher Capacitance, Higher energy
materials reaction and Electro chemical double density, Higher stability, Moderate
for the electrodes layer mechanism power density, Lower cyclic life.

Symmetric type Same electrodes with same combination of Reversible Faradaic Moderate- high Capacitance,
composite materials. reaction and Electro chemical double Higher energy density, Higher
layer mechanism stability,
Moderate power density, Lower
cyclic life.

Battery Type Anode: Battery type Lithium intercalation and de- Cycle life is poor. Power Density is
electrode Cathode: Carbon intercalation mechanism as observed in comparatively low, Higher specific
battery capacitance and energy density
Applications
 Consumer electronics
 Buffer power
 Voltage stabilizer
 Energy harvesting
 Incorporation into batteries
 Street lights
 Military
 Railways, light rails and trams
 Buses
Advantages
• High energy storage as a result of
using a porous activated carbon
electrode to achieve high surface
area
• Low equivalent series resistance
• Efficient performance at low
temperatures
• Fast charge-discharge rate
Disadvantages
• Low voltage per cell (typical
values for EDLC is 2.7 V) hence
series setup is required
• Cannot be used in alternating
current and frequency circuits
 Conducting Polymers
 CPs have recently attracted considerable attention because of their invaluable
advantages in compositing with other electroactive materials.

 Conducting polymers show pseudocapacitive nature thus they store charge used
faradic reaction.

 On the other hand, conducting polymers do not have a high surface area, and thus,
the electrochemical performance of conducting polymer is considerably based on
solid-state diffusion, which is slow.

 Polythiophene, Polypyrole , Polyacetylene and Polyaniline are the most widey

known conducting polymers.

 PANI as CP is the most viable option for pseudocapacitive composite owing to its
environmental stability, high ionic conductivity, multiple oxidation states, cost
effectiveness.
Activated carbon
 Activated carbons can be made from various substances.
 One of the best way to utilize waste material for such purposes
as it aids to solid waste managment.
 Activated carbon can be made from rice husk, coconut shell,
bamboo , fruit peels, pine niddles etc
 Citrus fruit peels are one of the best source for activated carbon
preparation.
 Carbon nanomaterials provide a spacious scaffold for the
polymer to grow on, but their capacitive contribution is not as
much as pseudocapacitive materials such as conducting
polymers.
Asymmetric supercapacitors

 This type of supercapacitor utilizes both the advantages of

pseudocapacitive and EDLC type materials.

 Here we make both the electrodes from different kind of

materials.

 Combination of Reversible Faradaic reaction and Electro

chemical double layer mechanism
 Asymmetric supercapacitor Optimization
Parameters
The important requirements for the optimization of electrode materials include:

Long and stable cycle life (>105)

Minimal irreversible redox processes

High specific surface area

Thermodynamic stability for a large potential window of operation

Excellent morphology, pore size, particle size, and material distribution

Surface wettability

High electrical conductivity

Sufficient thermal conductivity to reduce heat build-up within cell

Strong mechanical properties

 Literature Survey
Material Electrolyte Specific No. of Capacitance Year
capacitance cycles retention
(F/g) (%)

PANI 0.5 M H2SO4 168.0 10000 91 2011

PANI 1 M H2SO4 503 2000 89 2014

PANI 1 M H2SO4 480 3400 ∼100 2012
PANI 1 M H2SO4 532 1000 88 2011
PANI 1 M HCl 141.4 1000 ∼100 2010
PANI PVA/H3PO4 890 1500 97.9 2011
PANI CCl3COOH 135.4 1000 93.2 2015
PANI 0.1 M Na2SO4 330 1000 80.7 2014
PANI Gel polymer 672 1000 88 2015
PANI Gel polymer 250 1200 ∼100 2015
PANI Nafion 269 3000 95.5 2013
PANI
2013
nanowires 1 M H2SO4 742 1800 ∼100
 Contd…
Material Electrolyte Specific No. of Capacitance Year
capacitance cycles retention
(F/g) (%)

Nanofibrous 2010
PANI 1 M H2SO4 839 2000 88
Nanofibrous 2006
PANI 1 M H2SO4 861 1500 89
1 M H2SO4 2013
Sulfonated PANI 408 3000 93.2
PANI-LiPF6 1 M Et4NBF4 2008
74 2000 ∼100
PANI-LiPF6 1 M Et4NBF4 2006
107 3000 95.5
2008
PANI-LiPF6 Polyolefin 115 1800 ∼100
0.5 M H2SO4 2010
PANI/C 380 2000 88
0.5 M H2SO4 2011
PANI/CNT 1486 1000 93.2
PVA/H3PO4 2009
PANI/CNT 1065 1000 80.7
0.1 M H2SO4 2014
PANI/MWCNT 440 1500 88
1 M H2SO4 2011
PANI/SWCNT 560 1000 ∼100
 Contd…
Material Electrolyte Specific No. of Capacitance Year
capacitance(F cycles retention
/g) (%)

PANI-20 wt% 1 M H2SO4

670 NR NR 2005
MWNTs
PANI-Ti 0.5 M H2SO4 NR
740 NR 2011

PANI-80wt% 2.0 M H2SO4 NR

158 NR 2010
graphene
PANI-50wt%  2.0 M H2SO4 NR
207 NR 2010
graphene
PANI-10wt%  2.0 M H2SO4 NR
320 NR 2009
graphene
MPANI/CNTs 1.0 M H2SO4 NR
1030 NR 2014

PANI/activated 4 M KCl NR
273 NR 2005
carbon (16 wt%)
MWCNT/PAni NR NR
328 NR 2007
PAni/SWCNT NR
485 NR 2004
NR
 Contd…
Material Electrolyte Specific No. of Capacitance Year
capacitance(F cycles retention
/g) (%)

CSA-PANI/RGO
1 M H2SO4 431 500 74 2014

Ppy/TiN/PANI
Polypyrrole/titani
um
nitride/polyaniline  NR 1471.9 NR NR 2016
coaxial
nanotube hybrid

NiO-GNS/PANI
Nano nickel oxide-
coated NR NR 2016
 NR 1409
graphene/polyanili
ne

PANI/Graphene
  965 NR NR 2014

Non-irradiated HCl
Gel polymer
doped PAni 259 NR NR 2017
electrolyte
 Contd…
Material Electrolyte Specific No. of Capacitance Year
capacitance(F cycles retention
/g) (%)

Irradiated HCl Gel polymer

220 NR NR 2006
doped PAni electrolyte
PANI/RGO 1 M H2SO4 431
NR NR 2014
   
PANI/CNF 1 M H2SO4 400–557
NR NR 2013
   
PANI/N-doped
0.1 M Na2SO4
CNTs 250 NR NR 2013
 
 
N-doped 1 M Na2SO4
carbon/PANI 75–113 NR NR 2014
asymmetric    
CNF/GO/PANI 1 M H2SO4 479
NR NR 2014
   
PANI
1 M H2SO4
nanorods/Grap 836 NR NR 2014
 
hene  
RGO/NiO /PANI (1000) 100
 NR 638   2017
(5000) 91
 Contd…
Material Electrolyte Specific No. of Capacitance Year
capacitance(F cycles retention
/g) (%)

PANI nanowires
1 M H2SO4
68 Wh/kg 742 1500 92 2005
16 kW/kg
Nanofibrous PANI 1 M H2SO4 861 2000 82 2010
Hydrogel-
1 M methane
Assisted PANI 703 NR NR 2009
sulfonic acid
Microfiber
Self-doped PANI
0.5 Na2SO4 408 NR NR 2012
on carbon cloth
Sulfonated PANI 1 M H2SO4 1107 NR NR 2017
PANI-HCl 1 M Et4NBF4 70 1000 57 2002
PANI-NWs/CC NR 1079 NR NR 2010
PANI/CF NR 188 NR NR 2011
PANI/C60
Covalent bonding
of PANI onto
para-  NR 776 NR NR 2012
phenylenediamin
 Contd…
Material Electrolyte Specific No. of Capacitance Year
capacitance(F cycles retention
/g) (%)

PANI/CNT NR 400 NR NR 2012

PANI/CNT NR 838 NR NR 2011

PANI/CNT NR 1100 NR NR 2012

PANI/SWCNT NR 502 NR NR 2010

PANI/SWCNT NR 707 NR NR 2010

PANI/SWCNT NR 236 NR NR 2012

PANI/SWCNT NR 234 NR NR 2011

PANI-NWs/SWCNT NR 410 NR NR 2011

PANI/MWCNT NR 560 NR NR 2010

PANI/MWCNT NR 522 NR NR 2011

PANI-NRs/MWCNT NR 568 NR NR 2012

PANI-LiPF6 Polymer 2000 ∼100
80 2002
Electrolyte
PANI-LiPF6 1 M Et4NBF4 107 3000 95.5 2002
PANI-LiPF6 Polyolefin 115 1800 ∼100 2003
0.5 M H2SO4 2000 88
PANI/C 380 2002
 Contd…
Material Electrolyte Specific No. of Capacitance Year
capacitance(F cycles retention
/g) (%)

PANI-NRs/MWCNT
NR 515 NR NR 2011

PANI/graphene
NR 375 NR NR 2011

PANI/graphene
NR 587 NR NR 2012

PANI/graphene NR 1126 NR NR 2010

PANI/graphene NR 641 NR NR 2011
PANI/graphene
NR 346 NR NR 2012

PANI/graphene NR 500 NR NR 2011

PANI
NR 623 NR NR 2012
NFs/graphene
PANI
NFs/graphene NR 480 NR NR 2010

PANI
NFs/graphene NR 526 NR NR 2012

PANI
NFs/graphene NR 301 NR NR 2011
 Contd…
Material Electrolyte Specific No. of Capacitance Year
capacitance(F cycles retention
/g) (%)

PANi/Acetylene 1 M KOH 732 5000 78 2019

black

GO/ferocene 1 M KOH 200 NR NR 2019

PANi/CNF 1 M Na2SO4 234 1000 90 2019

Mudstone/AC 1 M Na2SO4 155.6 NR NR 2019

RGO/La2O3 6 M KOH 156.25 500 78 2019

PANI with 1 M Na2SO4 70.2 1000 90 2021

varying HCl
conc

PANI/Carbon 2 M KOH 1044 3000 80.1 2020

aerogel
Research gap
 Carboxylic acid as dopant and acidic medium for polyaniline synthesis has
been studied.

 There is lack of studies showing optimization of acid to aniline monomer

ratio.

 There is no article where citrus peels extract is used for PANI synthesis the
way I intend to do as per my knowledge.

 Also the peels post extraction can be used for Activated carbon
preparation with different activation technique.

 Comparission of chemical activation long with thermal activation and only

thermal activation in asymmretric electrode system is not much studied.
Working Plan
Preparation of citrus limeta peels extract

Preparation of polyaniline using oxidative polymerization

Preparation of activated carbon by various activation techniques

Prepare asymmetric supercapacitor using both the above synthesized

materials

Optimization of various variables like ph of extaract ,aniline monomer along

with oxidizing agent that will give best material for supercapacitor electrode
Methodology for PANI
Preparation of Polyaniline
(Oxidative polymerization reaction)

Use citrus limeta extract precooled for APS

Aniline acidic/doping medium solution
precooled to precooled
0-5 °C to 0-5 °C
Magnetic stirrer
(Ice bath)

Dark green solution

Stir 2 hrs & Refrigerate for

24 hrs

Vacuum filtration

Drying 60 °C
Carbon Based Material

Ativated carbon based material

EDLC (Less specific capacitance)

Higher stability & reversibility Citrus limeta

peels, pine
niddles
Provides electrochemical
reversibility during
swelling & shrinkage Naturally available and
(charge-discharge) of PANI cheaper than Graphene,
CNT etc
Preparation of Activated carbon

Activation can be done by chemical and/or thermal mode

Thermally activated carbons are made by heating at very high

temperature in inerts atmosphere

For chemical activation the peels are presoaked in acidic/basic solution

before thermal activation

Chemical activation adds to higher surface area and better pore

distribution
Electrode preparation
 2 mg sample +1000 μL Isopropyl
alcohol+ 50 μL Nafion

60 μL of dispersion dropped on
carbon paper & dried at
atmospheric conditions
Contd…
Electrode

Making of Supercapacitors device

Cyclic stability testing

Optimization of various parameters for

better performance

Finding out the kinetics, mechanism & contributions of different

parameters to performance
List of Characterization Techniques

 XRD (X-Ray Diffraction)

 FTIR (Fourier-transform infrared spectroscopy)

 SEM(Scanning electron microscopy)

 XPS(X-ray photoelectron spectroscopy)

 BET surface analysis(Brunauer–Emmett–Teller)

 CV (Cyclic voltametry)

 GCD (Galvanostatic charge discharge analysis)

 EIS (Electrochemical impedance spectroscopy)

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