3.

3 Procedure followed for electrochemical measurements

1. Working electrodes (the one we discussed their preparation method above) were connected to
red wire of the channel-3 of the potentiostat, while blue wire was connected to platinum
counter electrode and the white wire was connected to standard SCE electrode as shown in
figure.
2. CV was conducted at various scan rates to know the behaviour of the electrode and to check
reversibility of the reactions.
3. Once the CV was completed. Galvanostatic charge- discharge was carried out at various
current densities being 1, 2, 3, 4 and 5 A/g for 2-3 repeated cycles at each current density.
4. All the files were named & saved properly like, Sample Name-Slurry Batch Name-Electrode
Number-Number of Electrochemical Repetition-Channel Number. For example, NiNC-B1-
E1-1-C03
5. The data was transferred from the BioLogic software to MS Excel where all the required
calculations were done.
6. The specific capacitance of the Ni(OH)2/NC, Ni(OH)2/C and Ni(OH)2 was calculated from
charge-discharge curves under discharging condition based on the below equation:

𝐶𝐷 × ∆𝑡
𝐶𝑠 =
∆𝑉

7. To get Rogone plot the plot between energy density(E) and power density the below
equations were used to calculate these two:

1
𝐸= × 𝐶𝑠 × (∆𝑉)2 × 3.6
2

𝐸
𝑃= × 3600
∆𝑡

Where Cs (F/g) is the specific capacitance, CD is current density(A/g), Δt is the discharge time in
seconds, ΔV is the potential change with in the discharging time in Volts, E is energy density in
Wh/Kg and P is power density in KW/Kg.
4. Results and Discussion:

The electrochemical behaviour of Ni-NC, Ni-C and Ni(OH)2 were investigated by cyclic
voltammetry(CV) and galvanostatic charge-discharge techniques in a three electrode cell with
standard colomel electrode as reference electrode and platinum as counter electrode in a 1 M KOH
aqueous electrolyte. Figure 4a shows cyclic voltammetry curves in potential in a potential range of -
0.2 V to 0.9 V at an scan rate of 10mV/s. The curve shows redox peaks in the range of applied
potential implying that capacitance is governed by faradic redox reactions. The anodic peak
conforms to the oxidation of Ni(OH)2 to NiOOH while the cathodic represents the reduction of
NiOOH back to Ni(OH)2. The reaction occurring is shown below:

Ni(OH)2 + OH- NiOOH + H2O + e-

If we compare the three CV curves in Figure 4a, we see the CV curves of composites (Ni(OH)2/C
and Ni(OH)2/NC ) have both larger enclosed area of CV curves and an enhanced currents compared
to Ni(OH)2, which indicates that C and NC plays important role in enhancing pseudocapacitive
activity. This enhanced performance could be due to synergistic effect from Ni(OH)2 added. And
again, if we compare between C and NC, we see the peak separation is lesser in case of Ni(OH)2/NC
compared to Ni(OH)2/C composite demonstrating the improved utilization of electroactive species.

The capacitive performance was further investigated using galvanostatic charge-discharge technique.
Figure 4b shows the plot of specific capacitance of all three electrodes. A decrease in specific
capacitance with increasing current density is observed. This could be explained by the limited
diffusion of ions at higher current densities, that could only reach the outer active surface of the
electrode material for redox reactions.

On measurement of specific capacitance of three electrodes on the basis of discharge curves, the
specific capacitance of Ni(OH)2 obtained was lower than composites at each current density starting
from 1 A/g to 5 A/g. Initially, Ni(OH)2 had a very close capacitance being 1645 F/g for Ni(OH)2
and 1657 F/g for Ni(OH)2/C at 1 A/g which is because at lower current density the conductivity of
Ni(OH)2/C and Ni(OH)2/NC (more towards EDLC) is lesser than Ni(OH)2 because of less amount
of conductive material present in composites compared to Ni(OH)2 (more towards faradic
capacitance). At current density of 4 A/g the capacitance were 602 F/g, 635 F/g and 851 F/g for
Ni(OH)2, Ni(OH)2/C and Ni(OH)2/NC respectively. Therefore, at 4 A/g current density
Ni(OH)2/NC has 1.4 times more