Effective utilization and characterization of carbon

derived from non-biodegradable waste based

electrical switches for supercapacitor applications:
A green approach
Prabhin VS
T John Institute of Technology
BENITHA V S (  [email protected] )
Mepco Schlenk Engineering College
Jeyasubramanian K
Mepco Schlenk Engineering College
Shantha Selvakumari R
Mepco Schlenk Engineering College
Divya Divakaran
King Mongkut's Institute of Technology North Bangkok: King Mongkut's University of Technology North
Bangkok

Research Article

Keywords: Carbon, Char, DESTP, Supercapacitors, e-waste, Electrical switches, Specific capacitance

Posted Date: February 8th, 2023

DOI: https://doi.org/10.21203/rs.3.rs-2516296/v1

License:   This work is licensed under a Creative Commons Attribution 4.0 International License.
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Abstract
This work describes the utilization of carbon (Char) held after the slow pyrolysis of Disposed Electric
Switches made of Thermoset Plastic (DESTP) as a high-capacity electrode material for supercapacitor
applications. Char is prepared by pyrolysis strategy and exposed to severe milling in high energy
planetary ball mill for size reduction. By suspending the pulverised DESTP in silver (Ag) nanoparticles
dispersed solution obtained by reducing AgNO3 with hydrazine hydrate as a reducing agent, the DESTP is
loaded with Ag nanoparticles. The Energy Dispersive X-Ray Analysis (EDAX) validates the elemental
makeup of the manufactured char. The DESTP and Ag@DESTP are coated separately on a low-cost
etched brass substrate, and their electrochemical charge-storage properties are investigated using an
electrochemical workstation. The specific capacitance of DESTP and Ag@DESTP electrodes are
discovered to be 32 Fg-1and 67 Fg-1, respectively. The fabricated electrodes provide a maximum
volumetric capacitance of 93 mFcm-3and 21 mFcm-3 with a current density of 5 mA for Ag@DESTP and
DESTP electrodes respectively. This work gives a great model of repurposing the e-waste advertising with
good electrochemical energy storage applications.

1. Introduction
Innovations and technological advancements have resulted in significant changes in people's lives,
economies, and industries [1–5]. Simultaneously, this has resulted in a slew of issues, including the large
volume of hazardous garbage and other waste generated by electric products. E-waste is the fastest
developing squander stream, expanding at a disturbing rate which causes an irreversible effect on the
environment, on the off chance that legitimate strategies are not embraced for the transfer of these
wastes [6–9]. The rigorous use of polymer composites has caused environmental issues, since almost all
thermosetting plastics are non-biodegradable and possess lot of disposal limits [10, 11]. Despite this,
there is a significant increase in energy demand due to technological advancements, which is strongly
linked to rising levels of affluence and economic opportunity in much of the world [12–14]. Conversion
and storage of energy is clearly a crucial pillar of modern civilization, driven by the reciprocal promotion
of economic and environmental development.

Carbon-based supercapacitors are significant large-power devices that continue to dominate the
commercial industry, with features including millions of charge/discharge cycles, quick energy pulses,
wide range of operating temperatures, and high coulombic efficiency [15–18]. Because of their diverse
syntheses, outstanding physicochemical stability and electrical properties, porous carbons have become
a common electrode material in carbon based supercapacitors, it can also be generated from
conventional biomasses. Several researchers reported the use of carbon obtained from diverse
biomasses for supercapacitor applications [19]. Another reason for using such a new carbon normally
obtained from woods, barks, leaves, grasses, roots, etc. is owing to its availability and diversity of bio
resources. Recent advances in various ways of producing good performance, low-cost activated carbon
from respective renewable sources are discussed in the following sections.

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Yaglikciet al studied the performance of carbon supercapacitors made from waste tea and the
electrochemical performances were tested [20]. Fermanelliet al studied the carbon extraction from the
three types of biomass namely rice husk, peanut shell and wheat straw collected from agro industries, at
a pyrolysis temperature of 350–650°C. The study of pyrolysis temperature over the yield of bio-char,
liquid (bio-oil) and gaseous (bio-gas) fractions were evaluated for each biomass [21]. Jiangqi Zhou et al
studied about the biomass derived high capacitance super capacitors wherein they discussed about the
electrode materials with various nanostructures to augument exposed active surface areas, widen ionic
channels and accelerate electron conductivity [22]. Wenxin Hu et al prepared carbonaceous materials
from lignocellulosic biomass precursor which has the characteristics of low cost, natural abundance,
high specific surface area, and notable electrochemical stability [23].Another study revealed the use of
carbon coated core-shell nanomaterials for supercapacitor electrode [24].

In spite of the fact that customizing the geometrical morphologies, pore constructions, and surface
capacities in quest for enormous capacitance electrodes is featured in inventive carbon-based material
manufacture techniques, fostering another carbon is a new pushed region to store electrical energy in a
productive way [25]. From the writing, it is apparent that with the utilization of various kinds of carbon
derived from diverse biomasses are utilized for the manufacture of supercapacitor and its qualities were
advanced by various scientists [26–30]. Be that as it may, the utilization of carbon got from the pyrolysis
of thermosetting plastic widely utilized in the production of electrical appliances like waste electrical
switches as supercapacitor electrode materials are not announced up until this point.

Thus, in this specific situation, through this work a novel endeavour is made in regards to the devising of
carbon from squander electrical switches (disposed off into the municipal waste) by utilizing slow warm
pyrolysis. On heating the waste plastic at 400°C in an oxygen starved atmosphere yields about 60% of
carbonaceous content with 2.6% metallic oxides, which on subjected to size reduction by employing high
energy ball milling technique. The carbon acquired in 10 nm was additionally stacked with nano silver
particles by putting into a suspension having Ag nanoparticles got through the reduction of silver nitrate
utilizing hydrazine hydrate as a reducing agent. The dumped carbon (DESTP) and silver stacked DESTP
(Ag@DESTP) are utilized as electrode material in supercapacitor application. A supercapacitor electrode
with capacitance of 32 Fg− 1 and 67 Fg− 1 was attained by depositing DESTP and Ag@DESTP over an
etched brass substrate. This study paves the road for acquiring electrode material from waste and toxic
polymers that have been discarded into the environment.

2. Materials And Methods

Silver nitrate (AgNO3) and Sodium sulphate (Na2SO4) were purchased from Sigma Aldrich and was used
without any modification for depositing Ag over DESTP on brass substrate. Brass substrate with1 mm
thickness was purchased from the local Indian market and it was sized in the dimensions of 1 cm × 3 cm
as current collector. Before depositing Ag on the char, the substrate was cleaned by abrading with an
abrasive paper. The dirt particles were removed by washing with distilled water followed by sonicating in
acetone.
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2.1 Scrap material
Commercially available thermosetting electrical switches were collected from the municipal waste and
the metallic parts were removed manually. The non-metallic thermoset plastic was then cleaned with
distilled water to remove the dirt and manually crushed into small pieces.

2.2 Preparation of DESTP

About 5 g of waste switches were weighed and crushed into a fine powder mechanically. Then the
powdered sample was taken in a silica crucible, covered with a lid. This process not allows the intimate
mixing of air with the plastic powder. The contents were then heated at 400° C in a muffle furnace for a
period of 3 hrs. During heating, the organic contents present in the switches were decomposed in the
form of H2O (g), CO (g), etc., leaving2.44 g of carbon powder as a residue (approximately 50%). After the
pyrolysis, the carbon content retained on the crucible was grounded to a fine powder using pestle and
mortor. The same process was repeated to get bulk quantity of carbon powder from more amounts of
switches. About 20 g of powdered carbon was taken in a high energy ball mill (Fritsch, Germany) with a
powder to ball ratio of 1:10. The tungsten carbide balls were used to ground the carbon powder into nano
size and the milling process was carried outat a speed of 300 rpm. After 2 hrs of grinding, the obtained
carbon powder in nano size was collected and stored in vacuum.

2.3 Loading of nano Ag over carbon powder

About 0.01 M AgNO3 (1.70 g) was dissolved in 50 ml distilled water. Equimolar ratio of hydrazine hydrate
taken in 30 ml of distilled water was slowly added with constant stirring to the AgNO3 solution. After 3 hrs
of stirring, a yellow-colored solution was obtained confirms the formation of nano size silver particles.
Also, it was confirmed by recording UV spectra in which it exhibits a λmaxat 420 nm confirms the
formation of Ag nanoparticles[31]. After transferring the yellow color solution into a 250 ml beaker, 1 g of
nanosize carbon powder was slowly introduced with constant stirring. Addition of carbon powder was
continued for about 60 minutes. After 1 hr, settling of Ag@DESTP was noticed leaving a clear
supernatant liquid. This fact supportsthat the nano Ag particle were found adsorbed over the carbon
powder. Nanosize C and Ag loaded on C were also confirmed from FESEM with EDAX and XRD studies.

2.4 Fabrication of electrode

Low-cost brass substrate having composition of 66% Cu and 34% Zinc was used a current collector. The
porosity on the brass substrate was developed by soaking in 70% HNO3 for 5 seconds. During the
soaking process, the copper present in the brass substrate reacts with the acid and gets detachedout
leaving pores on the substrate. The brass substratewas then washedthoroughly with distilled water to
remove the traces of nitric acid adhered on thesurface. The cleaned substrate was preheated at a
temperature of 40°C in a hot plate. 0.01 g of DESTP and Ag@DESTP was individually dispersedin
acetone, wherein the uniform distribution of carbon powder and Ag@DESTP were obtained by sonication.
Then the respective suspensions weredeposited on the preheated substrate by drop casting method.
About 1 ml of the suspension containing carbon powder and Ag@DESTP were placed on the substrate
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kept over the hot plate maintained at 50–60°C. Complete dropping of 1 ml of the suspension produces
the carbon coated and Ag@DESTP coated electrodes.

3. Results And Discussion

3.1 XRD analysis
X-ray powder diffraction (XRD) is used for the analysis of phase purity and crystallinity of materials. XRD
patterns were captured from a Rigaku Ultima IV automatic multipurpose X-Ray Diffractometer (USA) with
Cu Kα radiation (λ = 1.5418 Å) operating at 40 kV with 30 mA current. Data were acquired in the range of
20° − 80° and the XRD peakscharacteristics to the prepared DESTP [Fig. 1(a)], consists of various peaks,
not all are originated from carbon. The diffraction peak obtained at 2θ = 27.15° (002) corresponds to the
carbon[JCPDS No. 08-0415]formed from the plastic waste[32]. In view of the fact that, during the
manufacture of electrical switches from bakelite, various additives were added to obtain the required
characteristics. The peak corresponding to 27.83° (110) and 63.96° (204) originated from TiO2[JCPDS
No. 71-1169][33], the peaks appeared at 2θ = 31.45°(100), 46.96°(102), 69.55°(201) were obtained from
ZnO[JCPDS No. 36-1451][34], the peak at 2θ = 39.34° (102) from SiO2[JCPDS No. 85–0335][35], the
peaks at 2θ = 55.12°(211) from BaO[JCPDS No. 89-8425][36]and a peak noticed at 2θ = 77.61°(311)from
Ag[JCPDS No. 04-0783][37]. The peaks originated from TiO2,ZnO,SiO2,BaO and Ag were due to the
presence of additives added while manufacturing and converted into their respective oxides during
pyrolysis. It is observed that, different oxides present in the DESTP were well matched with the
compounds present in EDAX analysis. It is observed that, due to the pyrolysis process, the depth of the
amorphous carbon peak becomes more exposed and moves to 26°-27°which is closely associated with
the processes of graphitization of the organic component and the development of the nanocrystalline
structure of the matrix[38, 39].

Figure 1(b) shows the XRD pattern of silver nanoparticles, in which the peaks appeared at 2θ = 38.26°,
44.44°, 64.61°, 77.55° are matched well with the Miller indices of (111), (200), (220), (311) reflections of
the face-centered cubic structure of metallic silver with the standard JCPDS card No. 04 0783 [37, 40].
Figure 1(c) is the XRD pattern of Ag@DESTP, in which all the peaks indexed in Fig. 1(a)is appeared along
with the silver peaks. This fact supports that the nano Ag particle were found loaded (adsorbed) over the
carbon powder and a decrease in the intensities is attributable to the Ag doping.

3.2 FESEM analysis

Field Emission Electron Microscope is used to examine the surface morphology and microstructure of the
obtained carbon and Ag loaded carbon. FESEM images are captured through FESEM-Carl Zeiss MA
15/EVO 18 electron microscope (Germany). The FESEM image of the brass and etched brass substrate
found after dipping in nitric acid is shown in Fig. 2(a) & (b). From Fig. 2(b), it is clear that the porous
nature of the brass substrate is because of the removal of Cu atoms from the brass substrate. The
reaction involved in the removal of Cu atoms is given in the Eq. 1.

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3 Cu + 8 HNO3 = 3 Cu(NO3)2+2 NO↑+4 H2O (1)
The porous structures are formed as a result of gas generation. Suchlike porous nature of the current
collector is more important in collecting and storing the charges. Figure 2 (c) depicts the porous structure
of DESTP with an average pore size of around 200 nm. The image also shows the dissection with trifling
and profound traps, which are significant for charge transportation and energy storage property [41, 42].
This geometry enhances the electrode surface area, leading to a rise in junction area between the
electrode material and the electrolyte. Figure 2 (d) shows the FESEM image of Ag@DESTP with a
mesoporous nature, and the particles are agglomerated and the individual particle is found to be in 10 nm
size.

Figure 3(a-d) is the EDAX analysis of brass substrate, etched brass, DESTP and Ag@DESTP respectively.
The EDAX clearly reveals the presence of Cu and Zn in Fig. 3(a) & (b) and the EDAX graph of DESTP and
Ag@DESTP (Fig. 3(c) & (d)) reveals the presence of C with other elements like Ti, Zn, Ba, Si, Ag as
confirmed from XRD. Various elements present in the brass substrate, etched brass substrate, DESTP &
Ag@DESTP with the atomic weight percentages are displayed in Fig. 4(a) & (b), from this it is observed
that around 4.27% of copper atoms have been etched from the substrate after immersion in 70% HNO3
for few seconds. The expulsion of copper atoms from the brass substrate paves a way for the better
adherence of DESTP and Ag@DESTP. Besides the conventional elements like Cu and Zn from the
substrate, after coating C, it exhibits a characteristic peak for carbon and nitrogen. In addition to these,
the EDAX clearly revealed the presence of atoms like Ti, Zn, Ba, Si which were all originated from the
additives. Interestingly, the Ag@DESTP additionally exhibits a characteristic peak for Ag, obviously
obtained from the loading of silver nanoparticles.

3.3 BET analysis

The porosity nature of the DESTP and Ag@DESTP materials is investigated using N2
absorption/desorption isotherms [Fig. 5(a) & (b)]. The behavior of N2 absorption/desorption resembles
that of a type IV isotherm including hysteresis. At low pressure, the adsorption and desorption isotherms
are superimposed, owing to the adsorption of gases in the micropores. As the pressure is increased, due
to the capillary agglomeration phenomenon, the isotherms increase rapidly forming a lag loop. The
surface area (SA) is vital for improving the performance and energy storage capability of the electrodes.
Employing BET analysis, the SA for DESTP and Ag@DESTP is found to be 238.98 m2 /g and 310.71
m2/g, respectively.

The pore size matrix of DESTP and Ag@DESTP are shown in Fig. 5c & d, which were calculated using the
BJH model. It is observed from the curve that the size of the pores are around 40 nm in DESTP [Fig. 5c]
and 6 nm in Ag@DESTP [Fig. 5d], attributing the presence of micropores.

3.4 Electrochemical analysis

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3.4.1 CV Analysis
Electrochemical investigations are carried out to measure the characteristics of the fabricated
supercapacitor electrodes. Each electrochemical study was performed via the electrochemical
workstation (CHI660C, USA). A standard three-electrode arrangement was used in this study consists of a
standard calomel cathode (SCE) as a reference electrode, platinum wire as a counter electrode and the
fabricated electrode as a working electrode respectively. All experiments were performed at room
temperature with 1 M aqueous sodium sulphate solution as the electrolyte. Figure 6 (a) & (b) shows the
CV curves of the DESTP and Ag@DESTP electrodes performed in a potential window of -0.8 V– 0V at
different scan speeds of 5,10, 25,50,75 and 100 mVs− 1 respectively. The CV curves show the significant
increase of specific capacitance after deposition of silver nanoparticles. From the voltametric profile, an
increase in the electric double layer capacitance is observed for Ag@DESTP electrode. The specific
capacitances of DESTP and Ag@DESTP electrodes were determined using the following equation [43–
45].

v1

Csp= (2)
1
∫ I (v) dv
mV (v2−v1)
v2

where, dv is the difference in potential, m is the mass of the electrode active material deposited, I(V) is the
current density, v is the scan rate in seconds and v1 and v2 are the cathodic and the anodic potential.

The mass of the active materials deposited over the etched brass current collectors were determined by
weighing the substrate before and after deposition of active materials employing digital balance. The
mass of the electrode active materials deposited over the electrode was 0.2mg and 0.23 mg in the case
of DESTP and Ag@DESTP electrodes respectively. The specific capacitance associated with DESTP and
Ag@DESTP electrodes are 32 Fg− 1 and 67 Fg− 1 with the scan rate of 5 mVs− 1 respectively. As the scan
rates are increased, the specific capacitance ofDESTP electrodes is decreased to 22, 16, 10, 8 and 5 Fg− 1
at the scan rates of and 10,25,50,75 and 100 mVs− 1 respectively. Eventually, the specific capacitance of
Ag@DESTP electrode is decreased to 36, 25, 16, 12 and 10 Fg− 1 at the scan rates of 10,25,50,75 and 100
mVs− 1 respectively. This outcome suggests a critical job that silver nanoparticles loaded on the
Ag@DESTP cathode significantly expanding the exposed surface area accessible for the greater
occurrence of the electric double layer process in an effective manner. A non-symmetric profile with
regards to the charging/releasing of the electric double layer is likewise observed. As indicated by the
cyclic voltammograms, the best behaviour of an electric double layer capacitance is appeared in the form
of a symmetric rectangular shape [46–48]. The deficiency of DESTP and Ag-DESTP electrodes
symmetricity might be related to conceivable reversible pseudo-faradaic responses that happened in a
likely area at around-0.6V and − 0.2 V. Furthermore, as electric double layer discharging happens, the
resulting current profile gets more inclined due to the fact that the ions leave the Ag pores with strain
most likely due to capillary effect [49–52]. Comparison of specific capacitance values of various
carbonaceous materials along with their data available is given in Table 1.

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 Table 1
Comparison of specific capacitance
Sl.No. Material Specific capacitance Reference

1 Graphene and carbon nanofiber (CNF) 51 Fg− 1 at 1 Ag− 1(CNF) [53]

409 Fg− 1 at 1 Ag− 1(MnO/CNF)

2 Carbon derived from areca fibres 34 Fg− 1 at 5 mVs− 1 (Non [54]

activated carbon)

64 5 mVs− 1 (activate carbon)

3 Hybrid fibers assembled from 20.7 Fg− 1 at a current density of [55]

MoSe2/grapheme heterostructures
0.1 A cm− 3(bare graphene
fibers)

135.1 Fg− 1 at a current density

of 0.1 Acm− 3 (MoSe2/graphene
hybrid fibers)

4 Carbonized PMF resin 58 Fg− 1 at 2 mVs− 1 (C700) [56]

5 Carbon derived from waste compact disk 51 Fg− 1 at 10 mVs− 1 [57]

which is activated by a single step process
of carbonization

followed by activation

Figure 7(a) & (b) show the galvanostatic charge discharge (GCD) curves of DESTP and Ag@DESTP
electrodes respectively. The pattern of the curve is not symmetrical in nature and the discharge time of
Ag-DESTP electrode is comparatively high, which proves its good charging capacity attributable to the
greater stacking of silver on the open-pores of the carbon. Moreover, the contribution of Ag nanoparticles
results in the large increase of electric double layer capacitance than pseudo capacitance which could be
noticed from the equivalent circuits of Ag@DESTP and DESTP. The double layer capacitance (Qdl) of
DESTP and Ag@DESTP obtained from equivalent circuit are 55 µF and 355 µF whereas, an increase of
diffusion capacitance Qd is not observed after incorporating Ag nanoparticles.

The hysteresis noticed in the charge discharge curve is due to IR drop in electrolyte resistance, change in
internal resistances and electrode materials [58–61]. The estimates of the IR drop from the DESTP and
Ag@DESTP electrodes were 0.25 V and 0.36 V respectively. A considerable increase in the IR drop of
Ag@DESTP electrode is attributed to the large surface area and volume change that occurs during Ag
doping process. Also, as the void spaces in the DESTP are filled by Ag nanoparticles, results in the
decrement in the contact spots of the etched current collector with the Ag@DESTP composite materials
owing to increase in IR drop of the electrode. Furthermore, the electrochemical characteristics were

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evaluated employing GCD curve recorded by the increasing current densities. It is obvious from the Fig. 7
(c) that the curve follows a diminishing specific capacitance trend as the scan rate increases. This is
explained by Randles-Sevcik equation in which, the current involved in the redox reaction is the square
root of the scan rate and linearly related to the concentration of the electro active substance. The Randle-
Sevcik equation is given below [62–64].

Ip=kn3/2AD 1/2Hf1/2 (3)

where, n represents the number of electrons, H is the solution concentration in moles/L, f is the scan rate
per time and D is the diffusion co-efficient in cm2. At lower scan rates, the dissemination of particles into
the interlayer of the electrodes happens subsequently, instigating a greater number of active sites for
charge-transfer responses [65, 66].

Figure 7(d) depicts the reduction of volumetric capacitance in analogous to the current density starting
from 5 mA to 7 mA in Na2SO4 electrolyte solution. The decrease in specific capacitance with the
augument in current density is because of the fact that, at higher current densities, the time taken for the
charging process is very less which leads to less ionic penetration at the surface of the electrode as
matched with low current density. The formula used to determine specific capacitance from GCD curve is
given in equation [67, 68].

iΔt
Cv =
vΔV

4
where, i is the charge current, Δt represents the discharge time, vis the effective volume of the electrode
and ΔV, the potential window (0V -0.8V). The electrodes provide the maximum volumetric capacitance of
93 mFcm− 3and 21 mFcm− 3 toward a current density of 5 mA for Ag@DESTP and DESTP electrodes
respectively. Figure 7(e) & (f) shows the specific capacitance retention of DESTP and Ag@DESTP
electrodes recorded at the sweep rate of 100 mVs− 1 for 5000 cycles. The electrodes retain the specific
capacitance of 93% and 91% of its initial values for DESTP and Ag@DESTP electrodes respectively.

The other vital parameters that affect the performance of supercapacitors are energy density and power
density. The Ed values of the supercapacitor electrodes could be analysed from the CV curves using the
following formula [69, 70]

2
C spV
Ed =
2

5
Where V is the potential window and Csp is the specific capacitance obtained from CV with scan rate of 5
mVs− 1. The power density is obtained by dividing the energy density by time taken toward the completion
of one periodic cycle using the expression [71].

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 Ed
Pd =
t

6
The energy and power density calculated from above expression for DESTP and Ag@DESTP electrodes
are 10.24 Wh/kg & 24.576 KW/Kg and 21.44 Wh/kg & 9.89 KW/kg respectively. Extraordinary power and
energy density in both the electrodes are attributed to the low inner resistance to charging and
discharging of electrodes which is replicated in EIS studies (Electrochemical impedance spectroscopy) as
well.

3.4.2 EIS Studies

Electrochemical impedance spectroscopy is a method used to determine the kinetic properties of the
active component’s as well as the electrodes capacitive nature. The resulting impedance is shown as real
and imaginary components of a supercapacitor as frequency dependent capacitance values [72, 73]. EIS
analysis was carried out over a DC voltage with a sinusoidal signal of small amplitude of 10 mV
spanning between the frequency of 0.1 Hz to 100 kHz.

Figure 8 (a) & (c) depicts the comparison between the Nyquist plot of DESTP and Ag@DESTP electrodes.
Figure 8(b) & (d) are the zoomed curves of Fig. 8(a) & (c), displaying the high frequency intersection of
Nyquist plot. The enlarged Nyquist plot attributes a quasi-semicircle type behaviour that is a non-vertical
line of intermediate frequency obtained by ion transport, restrictions in volumetric electrolyte transport,
ion transport routes from the volumetric electrolyte to the porous electrode surface caused by electrode
roughness and non-uniformity of the electrode pore size [74]. The intersection between the horizontal axis
and the vertical axis is aligned to the y axis at lower frequencies and is related to the frequency
dependent internal resistance and the equivalent resistance of the electrode [75–77]. The Equivalent
Series Resistance (ESR) of DESTP and Ag@DESTP electrodes are extracted from the intersection of the
real axis in the high frequency region of the Nyquist plot and are 28 Ω and 5 Ω, accordingly.

Furthermore, the Nyquist graph of the electrodes has two curve sections, one with 45° slopes that
intersects at higher frequency and a lower frequency region that depicts the component’s capacitive
behaviour. The capacity of the ions to infiltrate the pores at higher frequencies is largely limited, owing to
the electrodes repulsive behaviour. The curve shows a strong ramp of imaginary capacitance aligned to
the y-axis at the middle frequency, indicating good capacitance behaviour of the electrodes. The knee
frequency, which is associated with the initial frequency where electrolyte diffusion begins, is found at the
intersection of the intermediate and high frequency regions.The electrode extravagantly works as a
capacitor above the knee frequency, and its contribution to the specific capacitance is bigger in this time
scale.The knee frequency of DESTP and Ag@DESTP electrodes is 2 Hz and 9Hz, respectively, as shown in
Fig. 8 (b) & (d). For the DESTP and Ag@DESTP electrodes, the equivalent circuit gives values of 4.80 Ω &
1 Ω and 8.82 Ω &5.24 Ω for solution resistance Rs and Rct, which is the charge transfer resistance.

Page 10/28
Figure 8 (e) & (f) is the equivalent circuit design obtained for DESTP and Ag@DESTP electrodes, in which
the solution resistance Rs is connected to the other component since the current flows to the electrolyte at
different frequencies. The charge transfer resistance of Ag@DESTP was low owing to its higher
capacitance. The double layer charge is represented by the constant phase component Qdl. When the
frequency is reduced in the high frequency zone, the impedance provided by Qdl increases quickly,
allowing the current to pass through the charge transfer resistance Rct. The ion-desorption resistance of
DESTP and Ag-DESTP electrode materials is determined to be 21.05 Ω and 30.38 Ω, respectively.A
suitable electrode material must always have a high ion desorption resistance value. The current flows
through Rdes (desorption resistance) at low frequencies because the diffusion capacitance Qd has a very
high impedance. The diffusion capacitance value of the Ag@DESTP electrode is much larger than that of
the DESTP electrode, implying that the hybrid Ag@DESTP electrode has a higher specific capacitance
value.

The phase angle versus log frequency diagram, often known as the bode plot, depicts the impedance
characteristics of supercapacitors. Electrochemical nature of a supercapacitor varies between that of a
pure resistor with phase angle 0°and that of a pure capacitor with a phase angle of 90°. At higher
frequencies, the supercapacitor electrode behaves like a pure resistor since capacitance is inversely
proportional to frequency, resulting in a near zero impedance for a capacitor [78]. Figure 8 (g) shows the
phase angle vs frequency plot of DESTP and Ag@DESTP electrodes, with a maximum phase angles of
28° and 49°. The increase in the phase angle of Ag@DESTP is due to the enhanced faradaic contribution
of the electrode by silver particles. The time constant determined from maximum phase angle for DESTP
and Ag@DESTP are 1 s and 0.301 s respectively. Low time constant produced by Ag@DESTP electrode
have small time response which reveals the better performance of the supercapacitor electrode.

The capacitive characteristics of the electrodes are further investigated by utilising Equations (7 & 8) to
get the complex capacitances with respect to the given frequency [78].

−Z"
C’ω= (7)
ω× │Z"ω│2
′
−Z
C”ω= (8)
ω×│Z′ω│2

where, C’ω and C”ω are the real and imaginary capacitances and ω is the angular frequency. Figure 9(a) &
(b) depicts the real capacitance of the DESTP and Ag@DESTP electrodes respectively. In both the
electrodes, the real portion capacitance was initially large at lower frequencies and then gradually
decreased as the frequency increased. This could be influenced by the penetration of electrolytes into the
deep pores of the nanostructures at lower frequencies, while at higher frequencies electrolyte ions could
only reach the top surface materials. Figure 9(c) & (d) shows the imaginary capacitance of DESTP and
Ag@DESTP electrodes. The reciprocal of fo gives the dielectric relaxation time constant τo, and f is the
frequency at which the imaginary part capacitance reaches its highest value. The dielectric relaxation
time constants for DESTP and Ag@DESTP electrodes are 0.7 s and 0.1s, respectively, giving a similar

Page 11/28
time constant calculated from bode plot. Within this dielectric relaxation time constant fo, 50% of the
capacitance for the entire electrode system is achieved.

4. Conclusion
Based on the current study, the carbon obtained from the e-waste (thermoset plastic) was significantly
used as an energy storage material. Size reduction of the obtained char was done employing high energy
ball milling technique. The charge storing capacity of the carbon was further enhanced by loading silver
nano particles generated via wet chemical method. A simple drop casting method was adopted to coat
the DESTP and Ag@DESTP material on the low cost brass substrate. The findings reveal the prepared
electrode with etched brass substrate has a specific capacitance of 32 Fg− 1, yet on addition of Ag
significantly increasesthe specific capacitance to a value of 67 Fg− 1. Cyclic stability of the electrodes
was evaluated by running the cyclic voltammogram which displayed the retention of 93% and 91% for
DESTP and Ag@DESTP electrodes at the scan rateof100 mVs− 1 for 5000 cycles. Moreover, the results
obtained from the Nyquist and Bode plots of low solution resistance and time constant provide insight
into the reason for exceptional power density. This study focuses to achieve the recycling of carbon
obtained from e-waste (thermoset plastic) to be used as electrode material in supercapacitor. The
Ag@DESTP gave better performance after incorporating Ag nanoparticles and the results are advocated
by different characterization techniques like FESEM, BET, and CV. Following a comparison of these
samples with the literature, it is obvious that Ag@DESTP electrode performed respectfully in the area of
carbon-based composites. This in fact, encourages the fabrication of supercapacitor electrode using
DESTP-activated carbon.

Declarations
Acknowledgement:

The authors would like to thank the Principal and the Management of MEPCO Schlenk Engineering
College, Sivakasi for providing necessary experimental facilities to carry out this research work.

Ethical Approval

Not Applicable

Competing interests

The author(s) declared no competing interest with respect to the research, authorship, and/or publication
of this article

Authors' contributions

Page 12/28
V.S.Prabhin - Conceptualization, Investigation, Methodology, Writing Original Draft, Visualization and Data
Curation.

V.S.Benitha - Resources, Formal analysis, Validation, Writing - Review & Editing, Project Administration,
Supervision

K.Jeyasubramanian & R.Shantha Selvakumari - Visualization and Supported for data interpretation.

Divya Divakaran - Conceptualization, Writing - Review & Editing, Visualization and Supported for data
interpretation.

Funding

No funding is received for this research work.

Availability of data and materials

The data that support the findings of this study are available on request from the corresponding author.
The data are not publicly available due to privacy or ethical restrictions.

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Scheme
Scheme 1 is available in the Supplementary Files section.

Figures

Figure 1
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XRD pattern of (a) DESTP (b) Ag and (c) Ag@DESTP

Figure 2

FESEM images (a) Brass (b) Etched Brass (c) DESTP and (d) Ag@DESTP

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Figure 3

EDAX spectra (a) Brass (b) Etched Brass (c) DESTP and (d) Ag@DESTP

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Figure 4

Elemental composition of (a) brass and etched brass (b) DESTP and Ag@DESTP

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Figure 5

(a & b) N2 absorption/desorption isotherms of DESTP and Ag@DESTP and (c & d) BJH pore size
scattering plot of DESTP and Ag@DESTP.

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Figure 6

CV graphs recorded at different scan rates between 5 mVs-1and 100 mVs-1(a) DESTP and (b) Ag-DESTP.

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Figure 7

(a) & (b)Galvanostatic charge discharge voltage profiles between 5mA to 7 mA of DESTP and
Ag@DESTP electrodes, (c) & (d) Specific capacitance with respect to different scan rates between 5 mVs-
1
and 100 mVs-1and current density, (e) & (f) specific capacitance retention curves for DESTP and
Ag@DESTP electrode for 5000 cycles at the scan rate of 100 mVs-1

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Figure 8

EIS studies(a) & (c)Nyquist plot of DESTP and Ag@DESTP, (b) & (d) Zoomed image of(a) & (c), (e) & (f)
Equivalent circuit of Ag@DESTP and DESTP, (g) Phase angle plot of DESTP and Ag@DESTP electrodes.

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Figure 9

(a) & (b) Real capacitance of DESTP and Ag@DESTP electrode, (c) & (d) Imaginary capacitance of
DESTP and Ag@DESTP electrode.

Supplementary Files
This is a list of supplementary files associated with this preprint. Click to download.

floatimage1.jpeg

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