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Fabrication and characterization of Self-Supported NiCo-LDH

Arrays for High-performance Supercapacitor

Nixon Kiprotich

; Benard Kipsang

College of Mechanical and Vehicle Engineering, Hunan University, Changsha, 410082, China

Department of Advanced materials and technologies, Faculty of materials engineering, Silesian

University of Technology, 40-019, 08, Katowice

DOI:

https://doi.org/10.51583/IJLTEMAS.2026.1501000116

Received: 09 February 2026; Accepted: 12 February 2026; Published: 21 February 2026

ABSTRACT

Electrochemical capacitors have emerged as promising complementary energy storage systems to conventional

batteries due to their high-power density, rapid charge–discharge capability, and long cycle life. Extensive

research has focused on carbon-based electrode materials, which offer high surface area and good electrical

conductivity, enabling enhanced charge storage through electric double-layer mechanisms. However, despite

these advantages, the widespread replacement of batteries by electrochemical capacitors remains constrained by

limitations associated with electrode materials and fabrication methodologies. In particular, complex synthesis

routes, material costs, and scalability challenges continue to impede large-scale industrial deployment.

Consequently, the development of cost-effective materials and simplified fabrication strategies remains a critical

objective in advancing next-generation supercapacitor technologies. In this paper Nickel–cobalt layered double

hydroxide (NiCo-LDH) self-supported electrodes were fabricated via a cost-effective electrodeposition route on

hydrophilically treated indium tin oxide substrates for high-performance supercapacitor applications. Surface

roughening using potassium permanganate treatment enhanced wettability and effective surface area, while

subsequent nickel electroplating reduced substrate resistance from 34.4 Ω to 1.8 Ω, significantly improving

charge transport. Field-emission scanning electron microscopy revealed a hierarchical nanosheet morphology

with pronounced peaks and valleys, providing abundant electroactive sites for Faradaic reactions.

Electrochemical performance was evaluated in 2 M KOH using cyclic voltammetry, galvanostatic charge–

discharge, and electrochemical impedance spectroscopy. The electrode exhibited well-defined redox peaks

within a potential window of 0–0.55 V and delivered a high areal capacitance of 475 mF cm⁻² at 1 mA cm⁻²,

retaining 275 mF cm⁻² at 30 mA cm⁻² (42% retention). The small semicircle in Nyquist plots indicates low

charge-transfer resistance and efficient ion diffusion. Compared with previously reported carbon-based

electrodes and conventional NiCo-LDH systems, the present electrode exhibits competitive areal capacitance

and improved conductivity through direct current collector integration. The combination of simple fabrication,

reduced internal resistance, and stable electrochemical behavior highlights its potential for scalable industrial

energy storage applications such as backup power systems and hybrid capacitive devices.

Keywords: Nickel-cobalt layered double hydroxide; Self-supported electrodes; Electrodeposition;

Electrochemical capacitor, Supercapacitors, cyclic stability.

INTRODUCTION

Electrochemical capacitors have been achieved due to the ever-increasing need for energy by the population.

The research and development of an electrochemical capacitor began with the invention of a Leiden Jar which

yielded a capacitor which is a device that stores electrical charge in small quantities i.e. microfarads

[1].

Capacitors play a crucial role in electrical and electronic appliances since they are used in rectification, backup

circuits of the microcomputers, and timer circuits making use of periods to either charge or discharge electricity.

Capacitors are also applied to block the flow of direct current in filters responsible for extracting or eliminating

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specific frequencies. These circuits are applied on circuits where excellent frequency characteristic is a

requirement [2]

[3]

[4]

[5].

The advancement of technology in 21

century has given rise to the application of supercapacitor due to high

demand of portable and wearable devices. Electrochemical capacitor is made up of an electrolyte material

sandwiched between two identical electrodes. It stores electrical energy in the form of an electrochemical double

layer which is created at the interface of the solid electrode with either liquid or solid electrolyte. Both positive

and negative ionic charges present in the electrolyte materials accumulate at the surface of the electrode and

compensate for the electronic charges present at the surface of the electrode [6] [7]. The charging process of this

capacitor results in the alignment of opposite polarity charges in their respective opposite charge electrodes, ions

present in the electrolyte diffuse over the separator and onto the pores of the electrode with opposite charge or

polarity. Ions are prevented from recombining at the electrodes using a double layer of charge that is created in

the process. Combining both double layers results in an increase in the specific surface area, and the distance

between electrodes results in EDLCs attaining high energy density [2] [8].

The mechanism used by EDLCs to store electrical charges makes it possess a feature such as fast energy uptake,

delivery, and better power performance compared to other types of electrochemical capacitors. Because of the

non-faradaic process, swelling that is common in an active material demonstrated by a battery during charging

and discharging is eliminated. EDLCs and batteries vary from each other in few ways, for instance, EDLC can

undergo millions of charge-discharge cycles compared to batteries which can withstand few thousands of such

charge-discharge cycles before it is replaced. Also, the charge storage mechanism in EDLC does not involve the

solvent of the electrolyte while in battery storage mechanism contributes to solid electrolyte inter-phase when

high potential cathodes are used or graphite anodes [9] [10]. Even though EDLCs have better properties than

batteries, they experience a limited energy density thus explaining the reason why various recent research on

EDLC is focused on increasing energy performance and improving the temperature range where batteries cannot

operate. The performance of an EDLC is adjusted based on the type of electrolyte used.

Since the commercialization of ECs in the 1960s, there has been a lot of research work aimed at improving their

performances. Materials used in fabricating ECs play a vital role in the amount of capacitance it can store.

Materials of an EC are substrate-supported, implying that more than one material with different properties can

be combined using a specific method

[11]. For this reason, most of the research has focused on the best materials

that can produce an EC or supercapacitor with better performance and the method in which the same materials

are brought together to make up a supercapacitor or EC. In this section, therefore, the previous research work

will be discussed. It will be categorized into two parts, that is.; the research focused on materials.

In the research done by

[12] and [13], they found that the energy density of an EC can be increased by making

use of its specific surface area through wettability improvement [14] [15]. A highly flexible supercapacitor

electrode synthesized using the electro-deposition method was done. In their paper, manganese (IV) oxide was

electrodeposited onto carbon cloth designed using the facile in-situ electrodeposition method. From the

successfully synthesized electrode, it showed high flexibility with multiple layers structures which possessed

very high specific capacitance 325Fg

-1

at a current density of 0.2Ag

-1

and an excellent rate capability with

capacitance retention of 70% at a high current density of 5.0Ag

-1

[16],

In a work published in [17], an attempt was made to synthesize a flexible supercapacitor using nano-carbons,

manganese (IV) oxide, and PEDOT: PSS fibers. The team synthesized the flexible fiber supercapacitor by wet-

spinning using carbon nanotube. The surface treatment was deposited manganese (IV) oxide and PEDOT: PSS

onto the substrates to make the ternary composite fibers. Their research found out that by coating the fibers after

the wet spinning step, a simple solution-based continuous process results in forming a fiber-based energy storage

device.

Xing et al., 2017 [18] investigated the potential use of nickel-cobalt layered double hydroxide as a battery-type

hybrid supercapacitor. This material has a unique spatial structure, excellent electrochemical activity and good

electrical conductivity. However, this material is associated with challenges such as low electronic conductivity

resulting in low capacitance. [18]. An investigation aimed at optimizing the electrode preparation methodologies

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to realize the superior performance of supercapacitor through a rigorous understanding of underlying physical

parameters [19].

Zhang et al., 2014

[20] team, conducted a study on Nitrogen-doped hierarchically porous carbon Nano-whisker

ensembles on carbon nano-fiber for high-performance supercapacitors.

They combined surfactants and template less wet chemical and post-high-temperature carbonization strategies

for obtaining a new class of nitrogen-doped hierarchical porous carbon nano-whisker ensembles supported on

carbon Nano-fibers (NHCNs) with tunable micro-pores and a nitrogen-doping level for high-performance

supercapacitors [20].

In their work, Patrice et al. (2009) investigated the materials suitable for supercapacitor applications. They noted

in their research that supercapacitors have the potential of replacing batteries as energy storage devices.

A notable performance improvement could be achieved through recent advances in understanding charge storage

mechanisms and the development of advanced nanostructured materials [21].

Kim et al., 2015

[22] in their research on the electrochemical capacitor for energy storage and conversion,

acknowledge the fact that EC has the potential of replacing a lithium-ion battery in the future. Their work was

focused on analyzing the current trends in the research and development of EC and the challenges that are

currently preventing ECs from replacing the batteries fully entirely.

Their findings acknowledged that supercapacitors have better properties such as instant charging and discharging

with high power and retaining their performance for many million cycles compared to the batteries [23].

With the good properties of N-doped carbons, including their high electronic conductivity, improved hydrophilic

properties and easy syntheses and functionalization, Deng et al., 2016

[24] reviewed the potentiality of N-doped

carbons in energy storage and conversion applications.

Their work focused on the methods of preparations and their applications in supercapacitors in the past six years.

Their review study, found out that N-doped carbons have been prepared in the lab using various strategies

ranging from simple heat-treatment of carbons with nitrogen-containing complexes to carbonization of nitrogen-

containing complexes under an inert atmosphere or hydrothermal treatment.

During the preparation and heat treatment, it was clear that the strategies that result in high nitrogen content tend

to result in a low surface area, while the strategies that lead to an increase in the surface area resulted in a

reduction in nitrogen content.

The barrier responsible for the same challenges were attributed to the lack of effective methods to be used in

precisely controlling and obtaining ordered porous structures of N-doped carbons Efforts should be focused on

the control of the nature of nitrogen content in N-doped carbons for tunable electronic or chemical properties

and lack of scalable and inexpensive N-doped carbons preparation method [24].

Wang et al. (2016)

[25] reviewed the latest progress in supercapacitors in charge storage, electrode materials,

electrolyte materials, systems, characterization methods, and applications.

They mainly focused on the newly developed charge storage mechanism for inter-collative pseudocapacitive

behavior which connects the gap between battery behavior and conventional pseudocapacitive behavior and their

comparisons. They also touched on the prospects and challenges of supercapacitors in real-world applications.

They found that porous carbon materials are still widely used for electrode materials for ECs or supercapacitors.

Most of the previous research focused on optimizing the pore structure through the preparation of ordered and

hierarchical pores to improve the utilization of the pores.

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The diping process has been used to improve the specific Pseudo-capacitance. They also found that carbon

nanotubes and reduced graphene oxides show high electronic conductivity making it a suitable candidate for

flexible and printable supercapacitors [25].

From the above reviewed literature of recent publications there is still no simple and robust method and material

for use a capacitor electrode, therefor this work intends to describe a novel cost-effective electrodeposition

method for sizing NICOLDH based EC electrode.

Materials and equipment

The chemicals used in this research were sourced from Sinopharm Chemical Reagent (SCR) and they were of

analytical grade; thus, they were used without further purification.

METHODOLOGY

The fabrication involved two main steps, the preparation of current collectors and active materials. The current

collectors' preparation was done by first conducting hydrophilic treatment on the substrate. After this process,

the preparation for the electrodeposition plating solutions was done.

The solutions were categorized as solutions A, B, C, and D. Solution B comprised palladium (II) chloride and

hydrochloric acid. Solution C and D comprised of nickel (II) sulfate hexahydrate, citric acid monohydrate, nickel

(II) sulfate, and ammonium solution. Solution A was the last to be prepared because it is highly deliquescent. It

comprises stannous chloride and hydrochloric.

The indium tin oxide substrate was then prepared for electrodeposition by placing solutions A and B in their

respective beakers. Inside a water bath. After which, the indium tin oxide substrate was placed inside a beaker

with solution A for 10minutes, later removed and cleaned using deionized water, then dried.

The dried substrate was then placed inside a beaker with solution B for 15minutes, after which it was removed

and cleaned using deionized water and dried. The water bath temperature was raised to 70°C then a beaker

containing solution C and D was placed inside the water bath.

After this, the substrate was placed inside the beaker, and a vigorous reaction was allowed to take place for

3minutes then, the substrate was cleaned using deionized water then dried.

Finally, The current collectors' electrodeposition was prepared using nickel foam as a positive electrode (anode),

the substrate being the negative electrode and nickel sulfate as a plating solution.

The parameters were set accordingly on the ‘Kick Start’ software, The electrodeposition of current collectors

was done for 600 seconds, then the electrode substrate was removed and cleaned using deionized water then

dried. The characterization was done on the NiCo-LDH specimen using field emission scanning electron

microscopy.

RESULTS AND DISCUSSIONS

Solution Emersion using Potassium permanganate

Surface roughness plays a critical role in supercapcitor. For that reason, the surface area of the substrate was

increased by immersing it in potassium permanagnate solution which reduces the surface energy.

The process resulted in the increase in substrate’s surface roughness which directly contribute to an increase in

the specific surface area where the capacitance would be stored. Figure 3.1 shows a microscopic image of the

substrate surface after immesion in the potassium permanganate.To make the induced roughness on the

substrate’s surface permananent, the substrate was cleaned using plasma cleanr.

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Figure 3. 1: Microscopic image of the surface of the substrate after inserting it in potassium permanganate.

Electroplating.

Theoretically, a supercapacitor has small or negligible internal resistance. This was achieved during the

experiment through electro-depositing nickel on the hydrophilic treated electrode substrate using source meter

equipment. After inserting the electrode substrate in solutions A, B, C, and D, the resistance of the substrate

electrode was still high as shown by figure 3.2(a) i.e. 34.4Ω . The problem was solved by depositing nickel

metal onto the substrate ; the resistance decreased by 94.77%, as shown in Figure 3.2(b) i.e. 1.8Ω. As it is

evident in figure 3.2(c), the chemical deposited and electroplated nickels substrate is dull-grey while the

electrode substrate without nickel was shiny grey.

Figure 3. 2(a) Resistance before nickel deposition, figure 3.2(b) Resistance after nickel deposition, and figure

3.2(c) Comparison between the surface of the substrate electrode with and without nickel deposited .

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Nickel Cobalt Double-layered Electrode Hydroxide SEM Structure.

Figure 3.3(a), 3.3(b), 3.3(c), 3.3(d), and 3.3(e) show the microstructure of NiCo-LDH scanned at different

magnification factors. On the other hand, Figure 3.3(f) shows the NiCo-LDH optical microscope image.

As can be seen, the surface has peaks and valleys which contributes to an increase in the functional surface area

of the electrode which directly correspond to more capacitance being retained.

The rough surface of the NiCo-LDH structure indicates an improved contact angle within the microstructures.

This corresponds to an improved specific surface area utilization of the electrode.

An improved specific surface area utilization of the electrode, will result in a corresponding increase in the

amount of positive and negative ions that can accumulate on the surface of the electrode and thus improve

capacitance.

Figure 3. 3: Scanning Electron Microscopy images of NiCo-LDH.

Electrochemical characterization.

The characterization of the synthesized NiCo-LDH was done using electrochemical workstation using cyclic

voltammetry, chronopotentiometry, open-circuit potential, and specific capacitance as shown in Figure 3.4(a),

3.4(b), 3.4(c), and 3.4(d).

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Figure 3. 4 (a) CV curves at various scan rates inside 2M KOH electrolyte, figure 3.4(b) Charge-discharge

curves for NiCo-LDH in 2M KOH electrolyte at different current densities, figure 3.4(c) electrochemical

impedance spectroscopy in 2M KOH electrolyte and figure 3.4(c) Areal capacitance of NiCo-LDH in 2M

KOH electrolyte at different current densities.

Figures 3.4 shows the results processed using the chemistry workstation. The graphs play an important role in

interpreting the performance of the synthesized NiCo-LDH electrode.

The synthesized NiCo-LDH electrochemical supercapacitor electrode was characterized using electrochemical

workstation at various scan rates. As seen in Figure 3.4(a), the NiCo-LDH electrode specimen showed good

reversible redox reaction peaks falling in the range of -0.04Acm

-2

to 0.05Acm

-2

. This is attributed to the faradaic

redox reaction between nickel and cobalt ions as illustrated by chemical equations below.

𝑁𝑖

(

𝑂𝐻

)

+ 𝑂𝐻

−

↔ 𝑁𝑖𝑂𝑂𝐻 + 𝐻

𝑂 + 𝑒

−

𝐶𝑂

(

𝑂𝐻

)

+ 𝑂𝐻

−

↔ 𝐶𝑜𝑂𝑂𝐻 + 𝐻

𝑂 + 𝑒

−

𝐶𝑜𝑂𝑂𝐻 + 𝑂𝐻

−

↔ 𝐶𝑜𝑂

+ 𝑒

−

It can also be seen in Figure 3.4(a) that the NiCo-LDH electrode specimen had very high current peaks implying

that the charge transfer on the electrode specimen improved. The good redox reaction symmetry of the curves at

various scan rates implies that the NiCo-LDH electrode specimen has good electrochemical reversibility. It is

also clear from the same Figure 3.4(a) that the current peaks increase with the scan rates due to more diffusion

rates compared to reaction rate.

Figure 3.4(b) shows charge-discharge curve at different current densities;. 1mAcm

-2

, 2mAcm

-2

,5mAcm

-2

10mAcm

-2

, 20mAcm

-2

and 30mAcm

-2

. From the curve, the potential range between charging and discharging

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falls within 0V to 0.55V and is attributed to improved specific surface area utilization of the electrode substrate,

which in turn increases specific surface area utilization responsible for more capacitance. Also from the same

curve, the higher the current density, the lower the charging-discharging time and vice versa as evidenced by the

longer charging and discharging time for a current density of 1mAcm

-2

than a charging and discharging time for

a 30mAcm

-2

current density.

Electrode electrochemical impedance spectroscopy test was also carried out to investigate the impedance of the

resulting electrode. As shown in figure 3.4(c), the curve has a region of high frequency represented by half arc,

a region of intermediate frequency as represented by the transition section, and low frequency region represented

by the sizeable straight slope. The diameter of the half arch region shows the electrode and electrolyte surface

charge transfer resistance, while the small arc diameter represents the small or negligible electrochemical

impedance. On the other hand, the low-frequency region represented resistance of ion diffusion within the

material with larger straight slopes, a performance with similarities with an ideal capacitor.

Figure 3.4(d), illustrates that the amount of capacitance reduces as the current density increases. This is evident

by the falling curve with a reduction of 5.89%, 11.76%, 17.65%, 29.41%, 41.18% of capacitance for the current

densities of 1mAcm

-2

, 2mAcm

-2

, 5mAcm

-2

, 10mAcm

-2

, 20mAcm

-2

and 30mAcm

-2

respectively. The poor

capacitance retention of NiCo-LDH as the current density increases is attributed to its poor intrinsic conducting

nature otherwise, good capacitance retention at small current densities makes it good for industrial applications

such as energy power backups in computers, among others.

As discussed in the previous paragraphs, the synthesized supercapacitor based on NiCo-LDH shows an excellent

response to the application of various parameters. The results make the NiCo-LDH supercapacitor electrode a

suitable candidate for supercapacitor electrode applications. For instance, carbon-based electrodes have been in

applications for a long time. Now that there is a new material candidate, the reality of constructing a

supercapacitor that can store more electrical energy can be realized.

CONCLUSIONS AND RECOMMENDATIONS

The NiCo-LDH electrochemical capacitor electrode synthesized using the electrodeposition method was found

to show good reversible redox reactions, which in turn improved its faradaic reaction. The results exhibited an

improved charge transfer as evidenced by high current peaks and good electrochemical reversibility thus having

battery-like features.

The electrode was also found to retain more capacitance at lower current density.For instance, it could retain

425mFcm

-2

and 225mFcm

-2

at current densities of 1mAcm

-2

and 30mAcm

-2

, respectively. The charge-discharge

potential range of the synthesized electrode was 0.55V and this was contributed by improved wettability. All the

research objectives were achieved and thus, it was successfully done. The study recommend the use of NiCo-

LDH as a material for supercapacitor electrode applications.

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