Fabrication of Porous Ni-Co LDH Nanocomposites as Efficient Electrodes for Supercapacitors

Rosaiah, P.; Vadivel, S.; Prakash, Nunna Guru; Dhananjaya, Merum; Al-Asbahi, Bandar Ali; Roy, Soumyendu; Chalapathi, U.; Park, Si-Hyun

doi:https://doi.org/10.1155/2023/5793868

International Journal of Energy Research

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Abstract Introduction Experimental Results and Discussion Conclusions Data Availability Conflicts of Interest Authors’ Contributions Acknowledgments Supplementary Materials References Copyright Related Articles

Research Article | Open Access

Volume 2023 | Article ID 5793868 | https://doi.org/10.1155/2023/5793868

Fabrication of Porous Ni-Co LDH Nanocomposites as Efficient Electrodes for Supercapacitors

P. Rosaiah,^1,2S. Vadivel,²Nunna Guru Prakash,¹Merum Dhananjaya,¹Bandar Ali Al-Asbahi,³Soumyendu Roy,⁴U. Chalapathi,⁵and Si-Hyun Park⁵

Academic Editor: Pranav Kalidas Katkar

Received01 May 2023

Revised25 May 2023

Accepted02 Jun 2023

Published15 Jun 2023

Abstract

Nowadays, there is constant demand for the development of energy storage materials using advanced methodologies. In this scenario, a large-scale environmentally friendly synthesis was chosen to prepare Ni-Co-layered double hydroxide (LDH) composites for asymmetric supercapacitors. The developed materials had a flower-like porous architecture with very low dimensional layers and a large surface area. The developed Ni-Co/LDH composite electrodes showed impressive specific capacitance of 1095.1 F/g at a current density of 1 A/g and maintained 492.5 F/g even at a current density of 20 A/g. In particular, the Ni-Co/LDH composites maintained 86.9% of their initial capacitance even after 5000 cycles at a high current density of 2 A/g. Furthermore, an asymmetric supercapacitor with Ni-Co/LDH composites demonstrated an excellent energy density of 40.7 Wh/kg at a power density of 750 W/kg.

1. Introduction

The overwhelming human demand for renewable substances as well as the rapid development of human industrial applications constitutes significant challenges in terms of energy production and environmental protection [1, 2]. Scientists nowadays are well aware of the pressing need to emphasize research and development of energy conversion and storage devices to meet the growing demand. Due to their high power density and reliable cycling features, supercapacitors (SCs) have received a lot of attention from scientists in recent years [3, 4]. Morover, SCs also include the advantages of regular capacitors and rechargeable batteries to balance out their limitations [5]. Nevertheless, the commercial applications of SCs are limited by a number of factors that have a primary concern to scientific community. Consequently, the ultimate focus of SC technology is to increase the energy density of the SC by developing novel materials and methods [6]. In particular, the electrode materials in supercapacitors play a significant role in achieving remarkable energy densities and capacities. Since the composition and structure of materials influence their electrochemical properties, designing a compatible composition and structure can effectively boost the specific capacitances of electrode materials [7]. Therefore, substantial research has been undertaken recently to identify new SC electrode materials with superior properties [8]. For example, metal chalcogenides, polymers, and materials based on metal-organic frameworks have been employed to develop advanced SC electrode materials.

The inorganic layered materials termed as LDHs are composed of cationic brucite-like layers and exchangeable anions. LDHs can be formed by reacting most divalent and trivalent cations with appropriate anions [9, 10]. Transition metal LDHs have been receiving a lot of attention in the context of supercapacitor design because of their versatile chemical compositions, excellent anion exchange abilities, intercalating capabilities, and high redox activities [11, 12]. Due to their remarkable electrochemical qualities, LDHs based on Ni, Co, Mn, and Al have recently gained a lot of attention as SC electrode materials [13–16]. These metal LDHs have received particular attention in energy storage research because of their distinctive lamellar structures, large theoretical capacities, ease in fabrication, low cost, and environmental friendliness [17, 18]. Ni-Co/LDH composites have received the most attention among the various LDHs recently because of their improved conductivities and high capacitances with better cyclabilities [19, 20].

Despite the fact that there have been multiple publications on Ni-Co LDH, the rate capability and structural stability, particularly at high currents, are very poor, which is a major concern that needs to be addressed. Moreover, it is difficult to synthesize well-structured Ni-Co hydroxide composites due to the large difference in water solubility. Therefore, these concerns can be addressed by monitoring the surface architecture of the materials.

In the present study, we have chosen facile and cost-effective strategy to prepare flower-like Ni-Co/LDH nanocomposites. The solvothermally synthesized Ni-Co/LDH nanocomposites demonstrated competitive specific capacitance (Cs) of 1095.1 F/g at a current density of 1 A/g and maintained 86.9% of their initial capacitance even after 5000 cycles. Furthermore, the Ni-Co/LDH composite was used as the positive electrode in an asymmetric supercapacitor (ASC). This ASC displayed an excellent current density of 40.7 Wh/kg at a power density of 750 W/kg.

2. Experimental

Initially, 2.54 g 2-methylimidazole was dispersed in a 60 ml ethanol. Simultaneously, 2.2 g Co(NO₃)₂·6H₂O and 2.2 g Ni(NO₃)₂·6H₂O were dispersed in a 30 ml ethanol seperately. After proper stirring, these two solutions were dropped slowely into previous one. The resultant solution was then transferred to a 150 ml autoclave and proceed for solvothermal reaction. The reaction continued for 10 h at 70°C and then cooled naturally. After routine cleaning and proper drying, the resultant material was labelled 1 : 1, and further characterization was conducted. The other materials, such as 1 : 2 and 1 : 3, were also prepared with the same procedure, but their Co content was varied. Detailed experimental information was provided in the supplementary materials (available here).

3. Results and Discussion

The fabrication procedures for Ni-Co/LDH composites are depicted schematically in Figure 1. A facile and cost-effective strategy was used to prepare flower-like Ni-Co/LDH composites. The fundamental structural and surface characteristics of the Ni-Co/LDH composites were investigated using FE-SEM, TEM, XRD, and FT-IR. XRD patterns confirmed the crystallographic phase of the Ni-Co/LDH. Figure 2 displays the XRD patterns of Ni-Co/LDH composites in which all typical peaks were observed. These peaks were all in agreement with the JCPDS reference data (File No-040-0216) [21, 22]. It is observed that the diffraction peak around ° for the sample Ni-Co LDH (1 : 3) is shifted in comparison to the other samples. The other XRD peaks for Ni-Co LDH (1 : 3) also show conspicuous shifts towards higher angles. This is indicative of uniform compressive strain within the crystals of Ni-Co LDH (1 : 3). This could be due to the difference in sizes and bond lengths of Co and Ni atoms. The chemical functional groups present in a sample are examined using FT-IR spectroscopy. The FT-IR spectra of Ni-Co/LDH prepared at various concentrations are depicted in Figure 3. The FT-IR spectra of all materials exhibited three major peaks at 3472, 1382, and 638 cm^-1 which might be due to the coordinated H₂O molecules, asymmetric vibration of the group, and stretching vibration of metal oxide, respectively [23, 24]. The FT-IR spectra of composites prepared at various concentrations exhibited standard peaks, confirming the formation of the Ni-Co/LDH composite [25–27]. The chemical state and elemental composition of the Ni-Co/LDH were studied by XPS as shown in Figure S1. The XPS spectrum showed major peaks of O 1 s, Co 2p, Ni 2p, and N 1 s in their respective binding energy positions, indicating the structural integrity of the composites.

Figures 4(a)–4(f) depict FE-SEM images of Ni-Co/LDH prepared at 1 : 1, 1 : 2, and 1 : 3 concentrations. Even though, there is a flower-like morphology of all concentrations but not very clear for 1 : 1 and 1 : 3 concentration. Surprisingly, the composite materials prepared at 1 : 2 concentration displayed uniform-layered flower-like morphology. The surface morphology of the best sample (1 : 2) was further analyzed by TEM studies. Figures 4(g)–4(i) show the TEM, HRTEM, and SAED images of Ni-Co/LDH prepared at 1 : 2 tatio. The layered nanosheets are very thin and have a thickness of 10-20 nm. This type of architecture typically has a large surface area that further helps to improve electrochemical performance [28]. Furthermore, the composites show porous-like nature and low degree of lattice fringes (Figure 4(h)). The SAED pattern pointed on nanosheets also showed diffraction rings, indicating that the sample’s crystallinity is low (Figure 4(i)). Subsequently, the composite’s porosity was evaluated by N₂ adsorption/desorption experiments. Consequently, Figures 5(a)–5(f) show the N₂ adsorption/desorption isotherms and pore-size distribution profiles of Ni-Co/LDH composites, which displayed a type-IV hysteresis loop, demonstrating the mesoporous nature of these composites [29]. As illustrated in Figures 5(b), 5(d), and 5(f), the majority of the pore-size distribution could be observed within 20 nm. In addition, the estimated BET surface area of the Ni-Co/LDH composites synthesized at 1 : 1, 1 : 2, and 1 : 3 ratios was 37, 47, and 29 m²/g, respectively, demonstrating that the flower-like thin nanosheets were important in increasing the surface area of Ni-Co/LDH. Therefore, it is anticipated that Ni-Co/LDH composites synthesized at a ratio of 1 : 2 will demonstrate superior electrochemical performance.

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The electrochemical performance of Ni-Co/LDH materials was evaluated using CV and GCD experiments. Figures 6(a) and 6(b) show the CV (at 100 mV/s) and GCD (at 1 A/g) curves of Ni-Co/LDH composites synthesized at different ratios. Particularly, the scanned area of the Ni-Co/LDH (1 : 2 ratio) was much higher than that of other ratios (1 : 1 and 1 : 3), which might be because of the structural integrity and high surface area (Figure 6(a)). Moreover, GCD curves displayed higher discharge time, indicating the higher specific capacitance (Figure 6(b)). Figure 6(c) displays the CV profiles of the best sample (1 : 2 ratio) measured at a scan rate of 10-100 mV/s. As the scan rate increased, the CV profiles showed a shift in the direction of the corresponding potentials, indicating the presence of weak redox couples that originated from the Ni-foam. This changing behavior demonstrated the composites’ rapid redox reactions and high electrochemical reversibility [30]. In addition, the electrochemical redox reactions were described as [28, 31]:

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In order to comprehend about the composites’ electrochemical kinetics at different current densities, GCD experiments were conducted within the potential of 0 to 0.45 V. Figure 6(d) depicts the GCD curves of Ni-Co/LDH composites (1 : 2 ratio) cycled at various currents ranging from 1 to 20 A/g. The GCD profiles demonstrated that the composites had an outstanding charge/discharge behavior with an apparent pseudocapacitive characteristic [32]. Moreover, it demonstrated specific capacities of 1095.1, 991.0, 927.4, 825.8, 699.2, and 492.5 F/g, respectively, for current densities of 01, 02, 03, 05, 10, and 20 F/g (Figure 6(e)). Particularly, Ni-Co/LDH composites (1 : 2 ratio) showed a high specific capacitance (492.5 F/g) even at a high current (20 A/g), indicating an exceptional rate performance. Ni-Co/LDH composites synthesized at 1 : 1 and 1 : 3 ratio maintained a Cs of 453.1 and 387.6 F/g at 20 A/g. The porous-like nanosheets and high surface area promote high specific capacitance even at high currents, indicating the composites’ structural integrity [33, 34]. So, the Cs of the Ni-Co/LDH composites was better than that of other metal/metal oxide composites and similar LDH composites that have been reported in the literature. For example, Wang et al. synthesized the Co-Ni LDH nanosheets supported on Ni-foam which showed a specific capacitance of 774 F/g at 0.2 A/g, Wang et al. reported 708 c/g at 1 A/g, and Zhang et al. reported 381.3 F/g at 1 A/g. In Table S1, we present a comprehensive analysis of the findings of this study in relation to those of the published research [35–42]. Figure S2 depicts the capacitance and diffusion distribution curves of Ni-Co/LDH (1 : 2 sample), which clearly exhibited diffusion-controlled behavior.

Furthermore, GCD experiments were continued at high currents (2 A/g) for 5000 cycles in order to assess its long lifespan (Figure 6(f)). The cycling behavior of the Ni-Co/LDH was almost stable for 5000 cycles, with Cs of 881, 952, and 838 F/g for composites synthesized at 1 : 1, 1 : 2, and 1 : 3 ratios, respectively. In particular, the Ni-Co/LDH composite (1 : 2 ratio) preserved 86.9% of its initial capacitance, which was significantly higher compared to the other ratios. Ni-Co/LDH composites exhibit superior cycle performance and electrochemical stability as a result of their layered, interlaced nanosheets [43]. Furthermore, these results are superior to those reported for other metal/metal oxide and LDH composites [35, 38, 42]. The EIS studies were conducted to understand the inherent electrochemical kinetics of the sample. The EIS spectrum of 1 : 2 sample along with equivalent circuited is depicted in the inset of Figure 6(f), which exhibited low charge transfer resistance.

Meanwhile, a pouch cell supercapacitor device was assembled with the best sample (1 : 2) to comprehend the electrochemical behavior of Ni-Co/LDH composites (1 : 2 ratio) at the device level, and the corresponding supercapacitor device was termed as Ni-Co/LDH@SC (Figure 7(a)). The electrochemical behavior of activated carbon (AC) was tested within the potential range of -1 to 0 V, and corresponding CV and GCD curves were depicted in Figures 7(b) and 7(c). The GCD curve clearly exhibited triangular-shaped curves showing EDLC characteristics, with a Cs of 158 F/g at 1 A/g. Figure 7(d) shows the CV profiles of the Ni-Co/LDH@SC measured at different voltages while maintaining a constant scan rate of 50 mV/s. Figure 7(e) depicts CV curves of Ni-Co/LDH@SC recorded at best operating voltage of 0-1.5 V. As the scan rate increased from 10 mV/s to 100 mV/s, the shape of the CV curves changed significantly, indicating excellent rate capability. Moreover, GCD curves recorded at different currents maintained similar shape, showing better reversibility and high electronic transfer rate (Figure 7(f)). The Ni-Co/LDH@SC exhibited the Cs of 121.4, 100.0, 81.5, 72.3, and 60.4 F/g at current densities of 1, 2, 3, 5, and 10 A/g, respectively (Figure 7(g)). Specifically, even at a high current density of 10 A/g, it retained 50% of its initial Cs, suggesting an outstanding rate capability. In addition, these results are consistent with the scientific literature [44–46]. Since device-level cyclability is crucial, Ni-Co/LDH@SC was cycled at a high current density of 2 A/g for 5000 cycles, which sustained 78% stability with 97% of coulombic efficiency as shown in Figure 7(h), indicating excellent cycling stability and reversibility. The Ragone plots in Figure 7(i) depict the device’s energy and power densities. It is evident that the energy density maintained stable values as the power density increased, since the maximum energy density of 40.7 Wh/kg was maintained at a power density of 750 W/kg, which is significantly higher than that reported in the literature (Table S2) [44–52]. Furthermore, EIS spectrum of Ni-Co/LDH@SC is shown in Figure S3, which displayed low charge transfer resistance. As depicted in the inset of Figure 7(i), LED was activated with this device. These results indicate that the reported synthesis method is better suited for the preparation of high-performance electrodes even at the device level, and there is a lot of scope for further research to improve the capacitive behavior of the electrodes by doping them with different metals and conductive agents.

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4. Conclusions

In summary, the Ni-Co/LDH composites were synthesized using a facile solvothermal method. During the synthesis, Ni-Co/LDH composites exhibited flower-like surface architecture, with specific surface area ranging from 29 to 47 m²/g. The Ni-Co/LDH composites (1 : 2) displayed maximum specific capacitance of 1095.1 F/g at a current density of 1 A/g and maintained 492.5 F/g even at high current density of 20 A/g. The Ni-Co/LDH (1 : 2) composite was retained stable cycling stability for 5000 cycles, with a specific capacitance of 952 F/g which is 86.9% of its initial capacitance. Finally, an asymmetric pouch cell supercapacitor device was designed, with a maximum specific capacitance of 121.4 F/g at a current density of 1 A/g and a maximum energy density of 40.7 Wh/kg at a power density of 750 W/kg. In light of the high specific capacitance and exceptional cycling stability of the synthesized composites, this study demonstrates a facile method for fabricating superior electrode materials that are inexpensive and effective for high-performance supercapacitors.

Data Availability

Data will be available on request.

Conflicts of Interest

The authors declare that they have no conflict of interest.

Authors’ Contributions

PR conducted the conceptualization, methodology, and writing of the original draft. SV conducted the preparation and data acquisition. NGP and MD conducted the data acquisition and wrote, reviewed, and edited the paper. BA and SR conducted the data acquisition and reviewed and edited the paper. UC and SHP conceptualized and wrote the paper.

Acknowledgments

One of the authors (Bandar Ali Al-Asbahi) acknowledges Researchers Supporting Project number (RSP2023R348), King Saud University, Riyadh, Saudi Arabia.

Supplementary Materials

Supplementary information includes detailed experimental information. Table S1 &S2: comparison of the present work with the reported data. Figure S1: XPS spectrum of Ni-Co/LDH (1 : 2 sample). Figure S2: capacitance and diffusion distribution curves of Ni-Co/LDH (1 : 2 sample). Figure S3: EIS spectrum of Ni-Co/LDH@SC. (Supplementary Materials)

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Copyright © 2023 P. Rosaiah et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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