A Simple Method for Fabrication of Hybrid Electrodes of Supercapacitors

A Simple Method for Fabrication of Hybrid Electrodes of Supercapacitors | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Article A Simple Method for Fabrication of Hybrid Electrodes of Supercapacitors Samaneh Mahmoudi Qashqay, Mohammad-Reza Zamani Meymian, Ali Maleki This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-4414730/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 24 Nov, 2024 Read the published version in Scientific Reports → Version 1 posted 12 You are reading this latest preprint version Abstract The increasing need for electrode materials exhibiting improved performance to meet the requirements of supercapacitors is on the rise. Hybrid electrodes, which combine reduced graphene (RGO) oxide with transition metal-based oxides such as cobalt oxide (CoO), have emerged as promising materials due to their impressive specific capacitance and cost-effectiveness, attributed to their synergistic properties. In the present study, a binder-free RGOCoO composite electrode was synthesized using a facile, fast, and simple one-step co-precipitation method. This was done to improve stability for supercapacitor applications. The synthesized composite materials underwent comprehensive characterization utilizing various surface analytical techniques, including X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), field-emission scanning electron microscopy (FE-SEM), fourier-transform infrared spectroscopy (FTIR), and Brunauer–Emmett–Teller (BET) analysis. Electrochemical measurements of the fabricated hybrid revealed at current density of 2 A cm − 2 a specific capacitance of 132.3 mF cm − 2 , with an impressive 95.91% retention of capacitance after 7000 cycles. The results from electrochemical impedance spectroscopy (EIS) highlighted a meager low relaxation time constant of 0.53 s for the electrode. The reason behind this can be linked to the synergistic interactions, and minimal charge transfer resistance exhibited by the porous electrode without binders. The innovative simple synthesis of a binder-free RGOCoO composite electrode represents a significant advancement in the development of high-efficiency supercapacitors for diverse large-scale applications. Physical sciences/Materials science/Materials for devices Physical sciences/Chemistry/Electrochemistry Graphene Oxide Hybrid Cobalt Oxide Supercapacitor Inexpensive Facile Synthesis Relaxation Time Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Introduction The evolution of the global industry has spurred a demand for efficient, practical, and reliable electrochemical energy storage devices amidst the constant progress in new technologies such as wind systems, electric vehicles, and solar cells 1–9 . Supercapacitors have emerged as a cutting-edge energy storage solution, offering exceptional performance and contributing significantly to the global industry 10–12 . They are poised to lead the next generation of energy conversion systems, surpassing conventional energy storage devices like batteries, fuel cells, and capacitors due to their rapid recharge capabilities, high power density, extended lifespan, minimal maintenance requirements, adaptable packaging, and eco-friendly characteristics 13–16 . The selection of active electrode materials in supercapacitors profoundly impacts their electrochemical performance and energy storage capacity, making the quest for new electrode materials a critical aspect of supercapacitor development 17,18 . In the context of selecting an appropriate electrode material for supercapacitors, considerations include vital characteristics such as surface morphology, porosity, surface area, and electrical conductivity 19 . Three primary categories of electrode materials are commonly used in supercapacitor applications: metal oxides, carbon-based materials, and conductive polymers 20–22 . These materials possess distinct electrical, chemical, and structural properties that impact the overall performance and longevity of supercapacitors 23 . Carbon nanotubes and graphene exhibit superior conductivity, and graphene stands out as an exceptional electrode material due to its high electrical conductivity, flexibility, and large specific surface area 24–26 . Transition metal oxide and conducting polymer electrodes exhibit good energy density but have limited conductivity and cycle stability 27 . Therefore, the development of metal oxides with enhanced synergistic properties is vital 28 . To achieve high performance, a wide range of materials is applied in supercapacitor electrodes, often in combinations to create nanocomposite materials with versatile application capabilities 29 . Implementing chemical modifications on electrode materials with additional functional materials presents a practical method to produce tailored materials that enhance overall supercapacitor performance and display enhanced synergistic properties 30–32 . Recently, various approaches have been utilized for the advancement of electrode materials, such as hydrothermal/solvothermal processes, sol-gel methods, co-precipitation, chemical vapor deposition (CVD), ultrasonication, laser techniques, microwave routes, and more 33–35 . Among these, co-precipitation synthesis has emerged as a favored method due to its notable benefits, encompassing cost-effectiveness, high product yield with enhanced purity, fast heating, and efficiency in terms of time consumption 36–38 . Cobalt oxide (CoO), a vital transition metal oxide, holds significant promise in various fields such as lithium-ion batteries and heterogeneous catalysis due to its cost-effectiveness and environmentally friendly properties 39,40 . Recently, CoO has garnered attention in supercapacitors as an electrode material, showcasing potential as a cost-effective alternative to the widely utilized but expensive transition metal oxide 41,42 . Therefore, there is a pressing need for material scientists to explore simple and practical techniques for synthesizing the hybridization of CoO with highly conductive materials like graphene, which enhances electron transfer pathways and amplifies capacitance due to synergistic properties 43,44 . The internal resistance of a supercapacitor during operation is primarily composed of the ohmic, electron transfer, and diffusion resistances within the electrodes 45 . It is crucial to develop strategies for unraveling and examining the physical sub-processes and electrode kinetics of composite materials to enhance understanding and explore their performance and commercial viability further. Electrochemical impedance spectroscopy (EIS) is a vital tool for characterizing electrochemical systems, providing insights into various physical processes and chemical reactions, as well as interfacial phenomena occurring at different rates during electrode charging and discharging 46,47 . By employing relaxation time analysis, impedance spectra are transformed from the frequency domain to the time domain. This facilitates precise identification based on their characteristic time constants 48 . Considering the applicability of the relaxation time analysis for the evaluation of resistive-capacitive systems, but its limited exploration in the literature, this study provides a measurement of this case. Based on the literature review, we developed a simplified technique for producing a RGOCoO composite to serve as a promising electrode for supercapacitors. This study introduces a simple, fast, inexpensive, and effective technique that successfully yields RGOCoO electrodes through a precursor route, eliminating the need for surfactant, binder, and conductive additives. The objective is to leverage the synergistic properties of RGO, such as superior electrical conductivity, surface area, and chemical robustness, along with those of CoO, which features pseudocapacitive characteristics and enhanced energy storage capabilities. Apart from the usual structural and electrochemical characterization examinations, this study incorporates the performance kinetics of relaxation time based on the results obtained from EIS and delves into their underlying physical mechanisms. The RGOCoO hybrid demonstrates commendable electrochemical performance in terms of specific capacitance and cycling stability, showcasing its potential for advanced energy storage applications. Experimental details Synthesis of RGOCoO hybrid Graphene oxide was synthesized using a variation of the Hummer's method 49 starting from graphite powder, and subsequently reduced via hydrazine hydrate. To synthesize RGOCoO hybrid, 400 mg of RGO was mixed with 100 mL of deionized water and sonicated for 1 h to create a suspension. This suspension was then transferred to a flask and stirred in a water bath at room temperature. 100 mL solution of Co(Ac) 2 0.02 M was slowly added to the suspension. The mixture was stirred for several hours to ensure a complete reaction. Now, the final RGOCoO hybrid as slurry is ready to fabricate the supercapacitor electrode. Characterization Interfacial The analysis of the material's structure involved various techniques. A field emission scanning electron microscope (FESEM, MIRA3TESCAN-XMU) was used to observe the microstructure and atomic mapping. Crystallographic structure analysis was carried out using a powder X-ray diffractometer (XRD, Bruker D8 Advance) with Cu Kα radiation (λ = 0.15406 nm). Fourier transform infrared (FT-IR Spectrometer, Spectrum 100 (PerkinElmer USA) analysis was performed in the 4000 − 400 cm -1 region using KBr disks. In order to evaluate the specific surface area and porosity of the electrode material, an analysis based on the Brunauer-Emmett-Teller (BET, BELSORP –MiniX) method was performed. This involved determining the nitrogen (N 2 ) gas adsorption and desorption characteristics. Electrochemical Tests All electrochemical measurements were conducted on PGSTAT 204, Metrohm Autolab B.V., Netherlands employing NOVA 2.1 software electrochemical workstation. Electrodes were prepared by pressing a slurry onto a nickel foam current collector (1 cm × 1 cm) without useing binders and conductive additives, followed by overnight drying at 75°C. The specific capacitance of the supercapacitor was determined from the galvanostatic discharge curve by considering the total area of active materials on the electrode (A) as the following Eq. 5 0 : $$C=\frac{I\varDelta t}{A \varDelta v} \left(F{cm}^{-2}\right)$$ 1 The active area denoted by A is measured in cm², discharge time represented by Δt is calculated in seconds, the potential window indicated by ΔV, and the current denoted by I is measured in amperes (A). Electrochemical experiments were conducted using a three-electrode configuration with platinum foil as the counter electrode, an Ag/AgCl electrode as the reference electrode, and a 6.0 M aqueous KOH solution as the electrolyte. Results and discussion The surface morphology of the sample was investigated using FESEM. The FESEM image of CoRGO, as depicted in Fig. 1 a, reveals a bulky cluster containing RGO nanosheets with dispersed CoO nanoparticles. As illustrated in Fig. 1 b and 1 c, the ripple surface of RGO comprises ridges, wrinkles, and folds on both its upper and lower surfaces. The uniform distribution of CoO nanoparticles within the RGO nanosheets indicates the interactive an interactive nature, which assists in facilitating electron transfer, thereby enhancing the electrochemical performance. The presence of elements C, O, and Co was observed within RGOCoO by EDS analysis as shown in Fig. 1 S supplementary file that the atomic percentage composition of elements C, O, and Co in RGOCoO hybrid is 44.42%, 43.81%, and 11.77%, respectively. EDS mapping confirms the homogenous distribution of all elements (Fig. 1 d-g). The presence of C and O is attributed to the RGO nanosheet (Fig. 1 e and 1 f). In contrast, the presence of the Co, and O elements is attributed to the CoO nanoparticles (Fig. 1 f and 1 g). XRD analysis was performed to explore the structural and crystalline characteristics of the RGO and RGOCoO hybrid. In the XRD patterns, Fig. 2 . illustrates the peak at 26.5° corresponding to the (002) crystal plane in RGO. The XRD analysis of the RGOCoO hybrid reveals relatively weak diffraction peaks, suggesting the crystallized nature of CoO. The peaks observed at 33.31°, 42.20°, and 59.24° correspond to the (110), (200), and (220) planes, respectively, following the standard cubic structure of CoO (JCPDS No. 43-1004) 51 . Furthermore, the presence of RGO in the synthesized hybrid is confirmed by the peak at 26.50°, corresponding to the (002) plane. The utilization of FTIR Spectroscopy is pivotal for the development of the composites and hybrid to identify chemical bonds. Figure 3 illustrates the FTIR spectra showcasing IR bands for RGO and RGOCoO. The broad peak observed at 3434 cm⁻¹ in RGO can be ascribed to the stretching vibration of hydroxyl groups. The spectral features between 2840–2940 cm⁻¹ correspond to the C–H alkyl groups. Additionally, distinct IR bands at 1638 cm⁻¹, and 1577 cm⁻¹ are associated with the carboxylic acid stretching vibrations of C = O, and the alkenes stretching vibration of the C = C bond, respectively. Moreover, the peaks at 1168 cm⁻¹ and 1115 cm⁻¹ correspond to OH deformation and bending vibration, epoxy stretching of C-O-C, and alkoxy stretching of C-O, respectively. The FTIR spectrum of the RGOCoO hybrid reveals the vibrations of RGO and the attenuation of the hydroxyl group's broadband 52 . The spectrum of the RGOCoO hybrid manifests two distinct and intense peaks at 1568 cm⁻¹, 661 cm⁻¹ and 610 cm⁻¹, confirming the structure of CoO and the successful synthesis of the RGOCoO hybrid 53 . The structural properties of the surfaces, such as specific surface area, pore size distribution, and N 2 adsorption-desorption isotherms, are elucidated through BET analysis, as depicted in Fig. 4 a and b. A distinct hysteresis loop in the 0.4 − 1.0 P/P 0 range, indicating the N 2 adsorption-desorption isotherm of the electrode materials, closely resembling IV type with an H 3 hysteresis loop (Fig. 4 a). This observation indicates that the electrode materials possess a mesoporous structure. The RGOCoO shows a higher BET specific surface area of 59.59 m 2 g − 1 , accompanied by a pore volume measuring 13.69 cm 3 (STP) g − 1 compared to RGO with a specific surface area of 39.37, and a pore volume measuring 9.04 cm 3 (STP) g − 1 . Additionally, in Fig. 4 b, the Barrett-Joyner-Halenda (BJH) plot reveals an average pore diameter of 4.60 nm for the produced RGOCoO and 7.82 nm for RGO composites, affirming the presence of mesoporous in RGOCoO. The combination of a high BET surface area and porous characteristics enhances the reaction area, facilitating improved electrolyte penetration and efficient transport of electrons and ions within the electrode matrix, ultimately leading to enhanced supercapacitive performance attributed to the synergistic properties of CoRGO 54 . The straightforward fabrication process and synergistic properties position the RGOCoO hybrid as a promising candidate for applications in energy storage systems. To investigate the electrochemical performance of the RGOCoO electrodes, cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD) analyses were conducted in a 6 M KOH solution within a potential window of -0.1 to 0.45 V. The CV profiles of the RGOCoO and foam nickel were recorded at the scanning rate of 5 mV s⁻¹, illustrated in Fig. 5 a. The CV curve of RGOCoO exhibits a significantly larger area compared to that of foam nickel, indicating the negligible impact of foam nickel on capacitance. Figure 5 b displays the CV curves of the RGOCoO at various scan rates ranging from 5 to 80 mV s⁻¹. The nearly rectangular CV shapes suggest excellent capacitive behavior of the RGOCoO hybrid, with asymmetry likely stemming from the combination of double-layer capacitance (EDLC) from RGO and pseudocapacitance characteristics from the redox reaction of CoO. The emergence of a pair of subtle redox in the CV profiles of the hybrid is attributed to the following chemical reactions. CoO + OH − ↔ CoOOH + e − ( 2 ) CoOOH + OH − ↔ CoO 2 + H 2 O + e − ( 3 ) GCD measurements of the RGOCoO were conducted at different current densities, as depicted in Fig. 5 c, with specific capacitances calculated from the corresponding discharge profiles. The RGOCoO hybrid demonstrates good capacitive performance, as illustrated in Fig. 5 d, yielding specific capacitances of 132.3 mF cm − 2 at 2 mF cm − 2 . As the current density decreased, the capacitance values showed a notable increase. The reduction in specific capacitance as the current density increases can be elucidated as follows: The extended interaction duration between electrolyte ions and the RGOCoO electrode under low current density enables the accumulation of a significant charge quantity within the electrode, resulting in a high specific capacitance; and conversely, under high current density, the period of interaction between the electrolyte ions and the electrode is restricted. Consequently, a decreased specific capacitance is observed at higher current densities 32,55 . The cycling stability of the RGOCoO electrodes was assessed through charge/discharge cycling at a current density of 9 A cm⁻ 2 . After 7000 cycles, as exhibited in Fig. 5 e, the capacitance retention of the RGOCoO hybrid remains as high as 95.91%, indicating remarkable electrochemical stability. The investigation of capacitive elements and charge transfer kinetics of the RGOCoO electrode was conducted using EIS, performed in a 6 M KOH solution across the frequency range of 10 − 2 to 10 5 Hz. The EIS spectra of RGOCoO in Fig. 6 a display a linear trend with slight curvature in the higher frequency region, reflecting lower charge-transfer resistance and enhanced conductivity based on the Nyquist plot analysis. This improved performance can be attributed to the crumpled RGO sheets and the uniform dispersion of CoO spheres 56 . In the Bode plot illustrated in Fig. 6 b, the magnitude of total impedance |Z| decreased as the frequency increased. The resistive impedance shows minimal dependence on the frequency at 10 Hz and beyond. Figure 6 c illustrates the correlation between the phase angle and frequency, indicating the notable capacitance effect at lower frequencies (54.32°). The relaxation time constant (τ) required to discharge more than 50% of the total energy at an angle of approximately 45° is the minimum discharge time 57 . $$\tau =\frac{1}{2\pi {f}^{*}}$$ 4 Here, specific frequency f* corresponding to a phase angle of 45° equates to a time constant of τ = 0.53 s. This frequency marks the equilibrium point where the resistive and capacitive impedance components balance, leading to a shift towards a more resistive behavior in the supercapacitor at frequencies exceeding f*. This short time constant indicates a strong rate capability of the fabricated electrode material. In the AC response, the capacitor enters a complex domain that includes a real component C′(ω) and an imaginary component C″(ω) $$C\left(\omega \right)={C}^{{\prime }}\left(\omega \right)+iC{\prime }{\prime }\left(\omega \right)$$ 5 $$C{\prime }\left(\omega \right)=\frac{-{z}^{"}\left(\omega \right)}{\omega \times {\left|Z\left(\omega \right)\right|}^{2}}$$ 6 $$C{\prime }{\prime }\left(\omega \right)=\frac{-{Z}^{{\prime }}\left(\omega \right)}{\omega \times {\left|Z\left(f\right)\right|}^{2}}$$ 7 where the total capacitance is denoted by |C(ω)|² and \(\omega =2\pi f\) . The total impedance magnitude, real part (Z'), and imaginary part (Z'') are denoted as |Z|, Z', and Z'', respectively. In Fig. 6 d, the plot illustrates the relationship between real capacitance and real resistance, defining the charging behavior of the electrode. The activated material displayed an increase in resistance as capacitance increased. This phenomenon can be attributed to the penetration of the AC signal into pores of different sizes, resulting in the stabilization of capacitance levels. The imaginary and real components of capacitance are depicted in Fig. 6 e and f, illustrating a decrease in capacitance with increasing frequency. There is a decreasing trend from a frequency of 0.01 Hz to 10 Hz, while the trend remains constant at frequencies higher than 10 Hz. Ideally, pure capacitance possesses no real part as it contributes solely to power, while the imaginary part of capacitance, C″(ω), accounts for energy dissipation in an irreversible process. The enhanced electrochemical properties of the RGOCoO electrode can be attributed to several factors, including the notably larger specific surface area of the RGOCoO hybrid, which plays a crucial role in increasing the electron transfer rate. The specific structure of the hybrid facilitates electrolyte access to the electrochemical sites, resulting in shorter diffusion paths for adsorbing ions. Moreover, the crumpled RGO with numerous wrinkles and folds can promote high electronic conductivity and provide more reactive sites. These characteristics accelerate ion and charge transport during the charge/discharge process, improving cycle life stability 56 . Conclusion To summarize, a facile one-step approach has been introduced for the to fabricate of the RGOCoO electrode, resulting in the crumpled RGO sheets being non-uniformly distributed alongside CoO spheres. Hybrid electrode RGOCoO, offer the advantage that they serve as electrodes independently, without requiring additional active components like binders or conductive additives. The CoO, when combined with the crumpled RGO, offers synergistic characteristics by skillfully blending pseudocapacitive and EDLC-type materials. Expanding the external surface area enhances the effective interaction with ions in the electrolyte, and optimizing the pore size to match the ion size maximizes capacitance. This configuration enhances the electrical conductivity of the RGOCoO hybrid, making it suitable for use as an electrode. The optimized RGOCoO electrodes exhibited a notable specific capacitance of 132.3 mF cm − 2 and a remarkable capacitance retention of 95.91% after 7000 cycles. The rapid energy release indicated by the relaxation time of 0.53 s highlights the exceptional rate performance of the RGOCoO based supercapacitor, demonstrating the efficacy of this nanostructured material for high-performance energy storage applications. Declarations Supporting Information An accompanying supplementary document has been provided for this manuscript, which includes supplementary EDS analysis. Author Contribution S. M.Q.: Research and experiments, main researcher, writing manuscript (https://orcid.org/0000-0002-5419-9209). M.R.Z.M.:Project lead, conceptualization, validation, reviewing, and editing (https://orcid.org/0000-0002-8802-807X). A.M.: Conceptualization, validation, reviewing, and editing (https://orcid.org/0000-0001-5490-3350). Acknowledgement We extend our sincere gratitude to our esteemed colleagues at the Materials and Nanotechnology Research Laboratory (MNT Lab). Additionally, we would like to thank the Iran Fuel Conservation Company (IFCO) for their valuable assistance. We sincerely acknowledge the support of the Iran University of Science and Technology (IUST) and express our gratitude to their Central Laboratory, Physics Laboratory Services, and Chemistry Laboratory Services for their invaluable contributions to this research endeavor. We are also thankful to the Iran High-Tech Laboratory Network (Labsnet) for providing the necessary research facilities. 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Energy 220, 119696 (2021). Qu, D. et al. Electrochemical Impedance and its Applications in Energy-Storage Systems. Small Methods 2, 1700342 (2018). Wu, W. et al. Supercapacitive properties of MnO2 and underlying kinetics by distribution of relaxation time method. J. Power Sources 474, 228667 (2020). Wang, H. et al. Electrochemical impedance spectroscopy applied to microbial fuel cells: A review. Front. Microbiol. 13, (2022). Quattrocchi, E. et al. A general model for the impedance of batteries and supercapacitors: The non-linear distribution of diffusion times. Electrochim. Acta 324, 134853 (2019). Chen, J., Yao, B., Li, C. & Shi, G. An improved Hummers method for eco-friendly synthesis of graphene oxide. Carbon N. Y. 64, 225–229 (2013). Raza, W. et al. Recent advancements in supercapacitor technology. Nano Energy 52, 441–473 (2018). Liu, W. et al. Co-CoO/ZnFe2O4 encapsulated in carbon nanowires derived from MOFs as electrocatalysts for hydrogen evolution. J. Colloid Interface Sci. 561, 620–628 (2020). Sadhukhan, S. et al. Studies on synthesis of reduced graphene oxide (RGO) via green route and its electrical property. Mater. Res. Bull. 79, 41–51 (2016). Bhattacharya, P., Joo, T., Kota, M. & Park, H. S. CoO nanoparticles deposited on 3D macroporous ozonized RGO networks for high rate capability and ultralong cyclability of pseudocapacitors. Ceram. Int. 44, 980–987 (2018). Huang, J. et al. Ultrahigh-surface-area hierarchical porous carbon from chitosan: acetic acid mediated efficient synthesis and its application in superior supercapacitors. J. Mater. Chem. A 5, 24775–24781 (2017). Rani, B. & Sahu, N. K. Electrochemical properties of CoFe2O4 nanoparticles and its rGO composite for supercapacitor. Diam. Relat. Mater. 108, 107978 (2020). Mathew, E. E. & Balachandran, M. Crumpled and porous graphene for supercapacitor applications: a short review. Carbon Lett. 31, 537–555 (2021). Beidaghi, M. & Wang, C. Micro-Supercapacitors Based on Interdigital Electrodes of Reduced Graphene Oxide and Carbon Nanotube Composites with Ultrahigh Power Handling Performance. Adv. Funct. Mater. 22, 4501–4510 (2012). Additional Declarations No competing interests reported. Supplementary Files Supplementarymaterial.pdf Cite Share Download PDF Status: Published Journal Publication published 24 Nov, 2024 Read the published version in Scientific Reports → Version 1 posted Editorial decision: Revision requested 16 Oct, 2024 Reviewers agreed at journal 28 Aug, 2024 Reviews received at journal 28 Aug, 2024 Reviewers agreed at journal 26 Aug, 2024 Reviews received at journal 05 Jun, 2024 Reviewers agreed at journal 19 May, 2024 Reviewers agreed at journal 19 May, 2024 Reviewers invited by journal 19 May, 2024 Editor assigned by journal 19 May, 2024 Editor invited by journal 19 May, 2024 Submission checks completed at journal 17 May, 2024 First submitted to journal 13 May, 2024 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-4414730","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Article","associatedPublications":[],"authors":[{"id":305790245,"identity":"832945f9-e1f3-49c7-a1df-004b9c7a6a40","order_by":0,"name":"Samaneh Mahmoudi Qashqay","email":"","orcid":"","institution":"Iran University of Science and Technology","correspondingAuthor":false,"prefix":"","firstName":"Samaneh","middleName":"Mahmoudi","lastName":"Qashqay","suffix":""},{"id":305790246,"identity":"d12e61f6-d208-431e-86a0-44cb82d88545","order_by":1,"name":"Mohammad-Reza Zamani Meymian","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAAzklEQVRIiWNgGAWjYBADHn5mGJMZnzpkLZLNQPIAKVoYDA7AtBAC5g3sDz/dqLkjY3ycx/jzBwY7eQZ23gd4tcgcYEiWzjn2jMfsMI+ZBJBj2MDMboBXiwTQNdI5bIfBWoAOY05gYGbD7zAJBsbm3zn/DvMYN/MYfzjAUE+MFmY26dy2wzwGzDwGQIcdJkYLG5t1bt9hHonDbGUSZwyOG7YR1sL++HbOt8P2/P2HN3+oqKiW5+c/hl8Lg/wDZB4wrAjYMQpGwSgYBaOAGAAA7kI00o1RCFEAAAAASUVORK5CYII=","orcid":"","institution":"Iran University of Science and Technology","correspondingAuthor":true,"prefix":"","firstName":"Mohammad-Reza","middleName":"Zamani","lastName":"Meymian","suffix":""},{"id":305790247,"identity":"ab422699-62a9-467a-ba56-282795e2f0f0","order_by":2,"name":"Ali Maleki","email":"","orcid":"","institution":"Iran University of Science and Technology","correspondingAuthor":false,"prefix":"","firstName":"Ali","middleName":"","lastName":"Maleki","suffix":""}],"badges":[],"createdAt":"2024-05-13 17:40:18","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-4414730/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-4414730/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1038/s41598-024-80243-2","type":"published","date":"2024-11-24T15:57:44+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":57626382,"identity":"22e8ac34-bc4f-440c-b5d0-55f5c5060505","added_by":"auto","created_at":"2024-06-03 14:03:20","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":1065689,"visible":true,"origin":"","legend":"\u003cp\u003eFESEM images at magnification (a) 5μm, (b) 2 μm, (c) 500nm, EDS mapping of elements (d) C, (e) O, (e) Co of RGOCoO hybrid.\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-4414730/v1/1c057986c7504c557ead09d4.png"},{"id":57626378,"identity":"40276169-3372-4169-b57b-ff9b98a4a945","added_by":"auto","created_at":"2024-06-03 14:03:20","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":19985,"visible":true,"origin":"","legend":"\u003cp\u003eXRD patterns of RGO and RGOCoO hybrid\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-4414730/v1/83f466be77b709108f714ff3.png"},{"id":57626380,"identity":"6f785ca2-104a-49db-a707-0b373a53832a","added_by":"auto","created_at":"2024-06-03 14:03:20","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":35882,"visible":true,"origin":"","legend":"\u003cp\u003eFTIR patterns of RGO and RGOCoO hybrid.\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-4414730/v1/dd5bfa746a7c225a47151ef8.png"},{"id":57626379,"identity":"31c95f9d-e4ec-48a7-b4c3-bde155a57d8a","added_by":"auto","created_at":"2024-06-03 14:03:20","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":37550,"visible":true,"origin":"","legend":"\u003cp\u003eBET surface area measurement (a) the N\u003csub\u003e2\u003c/sub\u003e adsorption-desorption isotherms and (b) the pore size distribution of RGO and CoRGO.\u003c/p\u003e","description":"","filename":"4.png","url":"https://assets-eu.researchsquare.com/files/rs-4414730/v1/63393a6b9227ccfe780f2648.png"},{"id":57626384,"identity":"30c821d9-25c3-4303-aa64-cd09bfb3ae37","added_by":"auto","created_at":"2024-06-03 14:03:20","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":101484,"visible":true,"origin":"","legend":"\u003cp\u003e(a) comparative CV of RGOCoO, and foam nickel (b) CV curves of RGOCoO, (c) GCD curves RGOCoO, (d) Specific capacitance vs current density of RGOCoO, and (e) Cyclic stability of RGOCoO.\u003c/p\u003e","description":"","filename":"5.png","url":"https://assets-eu.researchsquare.com/files/rs-4414730/v1/83373e273a6946c077c68df6.png"},{"id":57627051,"identity":"2181ee87-500c-4f12-97c6-58b31d4965ad","added_by":"auto","created_at":"2024-06-03 14:11:20","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":84968,"visible":true,"origin":"","legend":"\u003cp\u003e(a) EIS (b) Bode plot (c) phase angle curves (c) real part of capacitance versus frequency response (d) real capacitance versus real resistance (e) real capacitance versus frequency (f) imaginary capacitance versus frequency.\u003c/p\u003e","description":"","filename":"6.png","url":"https://assets-eu.researchsquare.com/files/rs-4414730/v1/95bdf42a7e9cc974260a134f.png"},{"id":69834910,"identity":"0c168bb1-4b8a-4526-afcb-b5ebc36ad723","added_by":"auto","created_at":"2024-11-25 16:10:18","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1683919,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-4414730/v1/cd4479f1-1851-438a-8da4-cdf5d330aa82.pdf"},{"id":57626383,"identity":"bc336985-0252-440c-ae6d-e4024021dac3","added_by":"auto","created_at":"2024-06-03 14:03:20","extension":"pdf","order_by":2,"title":"","display":"","copyAsset":false,"role":"supplement","size":193497,"visible":true,"origin":"","legend":"","description":"","filename":"Supplementarymaterial.pdf","url":"https://assets-eu.researchsquare.com/files/rs-4414730/v1/d971c8da607c494a0e81c9ff.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"A Simple Method for Fabrication of Hybrid Electrodes of Supercapacitors","fulltext":[{"header":"Introduction","content":"\u003cp\u003eThe evolution of the global industry has spurred a demand for efficient, practical, and reliable electrochemical energy storage devices amidst the constant progress in new technologies such as wind systems, electric vehicles, and solar cells \u003csup\u003e1\u0026ndash;9\u003c/sup\u003e. Supercapacitors have emerged as a cutting-edge energy storage solution, offering exceptional performance and contributing significantly to the global industry\u003csup\u003e10\u0026ndash;12\u003c/sup\u003e. They are poised to lead the next generation of energy conversion systems, surpassing conventional energy storage devices like batteries, fuel cells, and capacitors due to their rapid recharge capabilities, high power density, extended lifespan, minimal maintenance requirements, adaptable packaging, and eco-friendly characteristics \u003csup\u003e13\u0026ndash;16\u003c/sup\u003e.\u003c/p\u003e \u003cp\u003eThe selection of active electrode materials in supercapacitors profoundly impacts their electrochemical performance and energy storage capacity, making the quest for new electrode materials a critical aspect of supercapacitor development\u003csup\u003e17,18\u003c/sup\u003e. In the context of selecting an appropriate electrode material for supercapacitors, considerations include vital characteristics such as surface morphology, porosity, surface area, and electrical conductivity\u003csup\u003e19\u003c/sup\u003e. Three primary categories of electrode materials are commonly used in supercapacitor applications: metal oxides, carbon-based materials, and conductive polymers\u003csup\u003e20\u0026ndash;22\u003c/sup\u003e. These materials possess distinct electrical, chemical, and structural properties that impact the overall performance and longevity of supercapacitors\u003csup\u003e23\u003c/sup\u003e.\u003c/p\u003e \u003cp\u003eCarbon nanotubes and graphene exhibit superior conductivity, and graphene stands out as an exceptional electrode material due to its high electrical conductivity, flexibility, and large specific surface area\u003csup\u003e24\u0026ndash;26\u003c/sup\u003e. Transition metal oxide and conducting polymer electrodes exhibit good energy density but have limited conductivity and cycle stability\u003csup\u003e27\u003c/sup\u003e. Therefore, the development of metal oxides with enhanced synergistic properties is vital\u003csup\u003e28\u003c/sup\u003e. To achieve high performance, a wide range of materials is applied in supercapacitor electrodes, often in combinations to create nanocomposite materials with versatile application capabilities\u003csup\u003e29\u003c/sup\u003e. Implementing chemical modifications on electrode materials with additional functional materials presents a practical method to produce tailored materials that enhance overall supercapacitor performance and display enhanced synergistic properties\u003csup\u003e30\u0026ndash;32\u003c/sup\u003e.\u003c/p\u003e \u003cp\u003eRecently, various approaches have been utilized for the advancement of electrode materials, such as hydrothermal/solvothermal processes, sol-gel methods, co-precipitation, chemical vapor deposition (CVD), ultrasonication, laser techniques, microwave routes, and more\u003csup\u003e33\u0026ndash;35\u003c/sup\u003e. Among these, co-precipitation synthesis has emerged as a favored method due to its notable benefits, encompassing cost-effectiveness, high product yield with enhanced purity, fast heating, and efficiency in terms of time consumption\u003csup\u003e36\u0026ndash;38\u003c/sup\u003e.\u003c/p\u003e \u003cp\u003eCobalt oxide (CoO), a vital transition metal oxide, holds significant promise in various fields such as lithium-ion batteries and heterogeneous catalysis due to its cost-effectiveness and environmentally friendly properties\u003csup\u003e39,40\u003c/sup\u003e. Recently, CoO has garnered attention in supercapacitors as an electrode material, showcasing potential as a cost-effective alternative to the widely utilized but expensive transition metal oxide\u003csup\u003e41,42\u003c/sup\u003e. Therefore, there is a pressing need for material scientists to explore simple and practical techniques for synthesizing the hybridization of CoO with highly conductive materials like graphene, which enhances electron transfer pathways and amplifies capacitance due to synergistic properties\u003csup\u003e43,44\u003c/sup\u003e.\u003c/p\u003e \u003cp\u003eThe internal resistance of a supercapacitor during operation is primarily composed of the ohmic, electron transfer, and diffusion resistances within the electrodes\u003csup\u003e45\u003c/sup\u003e. It is crucial to develop strategies for unraveling and examining the physical sub-processes and electrode kinetics of composite materials to enhance understanding and explore their performance and commercial viability further. Electrochemical impedance spectroscopy (EIS) is a vital tool for characterizing electrochemical systems, providing insights into various physical processes and chemical reactions, as well as interfacial phenomena occurring at different rates during electrode charging and discharging\u003csup\u003e46,47\u003c/sup\u003e. By employing relaxation time analysis, impedance spectra are transformed from the frequency domain to the time domain. This facilitates precise identification based on their characteristic time constants \u003csup\u003e48\u003c/sup\u003e. Considering the applicability of the relaxation time analysis for the evaluation of resistive-capacitive systems, but its limited exploration in the literature, this study provides a measurement of this case.\u003c/p\u003e \u003cp\u003eBased on the literature review, we developed a simplified technique for producing a RGOCoO composite to serve as a promising electrode for supercapacitors. This study introduces a simple, fast, inexpensive, and effective technique that successfully yields RGOCoO electrodes through a precursor route, eliminating the need for surfactant, binder, and conductive additives. The objective is to leverage the synergistic properties of RGO, such as superior electrical conductivity, surface area, and chemical robustness, along with those of CoO, which features pseudocapacitive characteristics and enhanced energy storage capabilities. Apart from the usual structural and electrochemical characterization examinations, this study incorporates the performance kinetics of relaxation time based on the results obtained from EIS and delves into their underlying physical mechanisms. The RGOCoO hybrid demonstrates commendable electrochemical performance in terms of specific capacitance and cycling stability, showcasing its potential for advanced energy storage applications.\u003c/p\u003e"},{"header":"Experimental details","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003eSynthesis of RGOCoO hybrid\u003c/h2\u003e \u003cp\u003eGraphene oxide was synthesized using a variation of the Hummer's method\u003csup\u003e49\u003c/sup\u003estarting from graphite powder, and subsequently reduced via hydrazine hydrate. To synthesize RGOCoO hybrid, 400 mg of RGO was mixed with 100 mL of deionized water and sonicated for 1 h to create a suspension. This suspension was then transferred to a flask and stirred in a water bath at room temperature. 100 mL solution of Co(Ac)\u003csub\u003e2\u003c/sub\u003e 0.02 M was slowly added to the suspension. The mixture was stirred for several hours to ensure a complete reaction. Now, the final RGOCoO hybrid as slurry is ready to fabricate the supercapacitor electrode.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003eCharacterization\u003c/h2\u003e \u003cdiv id=\"Sec5\" class=\"Section3\"\u003e \u003ch2\u003eInterfacial\u003c/h2\u003e \u003cp\u003eThe analysis of the material's structure involved various techniques. A field emission scanning electron microscope (FESEM, MIRA3TESCAN-XMU) was used to observe the microstructure and atomic mapping. Crystallographic structure analysis was carried out using a powder X-ray diffractometer (XRD, Bruker D8 Advance) with Cu Kα radiation (λ\u0026thinsp;=\u0026thinsp;0.15406 nm). Fourier transform infrared (FT-IR Spectrometer, Spectrum 100 (PerkinElmer USA) analysis was performed in the 4000\u0026thinsp;\u0026minus;\u0026thinsp;400 cm\u003csup\u003e-1\u003c/sup\u003e region using KBr disks. In order to evaluate the specific surface area and porosity of the electrode material, an analysis based on the Brunauer-Emmett-Teller (BET, BELSORP \u0026ndash;MiniX) method was performed. This involved determining the nitrogen (N\u003csub\u003e2\u003c/sub\u003e) gas adsorption and desorption characteristics.\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003eElectrochemical Tests\u003c/h2\u003e \u003cp\u003eAll electrochemical measurements were conducted on PGSTAT 204, Metrohm Autolab B.V., Netherlands employing NOVA 2.1 software electrochemical workstation. Electrodes were prepared by pressing a slurry onto a nickel foam current collector (1 cm \u0026times; 1 cm) without useing binders and conductive additives, followed by overnight drying at 75\u0026deg;C. The specific capacitance of the supercapacitor was determined from the galvanostatic discharge curve by considering the total area of active materials on the electrode (A) as the following Eq.\u0026nbsp;5\u003csup\u003e0\u003c/sup\u003e:\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ1\" name=\"EquationSource\"\u003e\n$$C=\\frac{I\\varDelta t}{A \\varDelta v} \\left(F{cm}^{-2}\\right)$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e1\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eThe active area denoted by A is measured in cm\u0026sup2;, discharge time represented by Δt is calculated in seconds, the potential window indicated by ΔV, and the current denoted by I is measured in amperes (A). Electrochemical experiments were conducted using a three-electrode configuration with platinum foil as the counter electrode, an Ag/AgCl electrode as the reference electrode, and a 6.0 M aqueous KOH solution as the electrolyte.\u003c/p\u003e \u003c/div\u003e"},{"header":"Results and discussion","content":"\u003cp\u003eThe surface morphology of the sample was investigated using FESEM. The FESEM image of CoRGO, as depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ea, reveals a bulky cluster containing RGO nanosheets with dispersed CoO nanoparticles. As illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eb and \u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ec, the ripple surface of RGO comprises ridges, wrinkles, and folds on both its upper and lower surfaces. The uniform distribution of CoO nanoparticles within the RGO nanosheets indicates the interactive an interactive nature, which assists in facilitating electron transfer, thereby enhancing the electrochemical performance. The presence of elements C, O, and Co was observed within RGOCoO by EDS analysis as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eS supplementary file that the atomic percentage composition of elements C, O, and Co in RGOCoO hybrid is 44.42%, 43.81%, and 11.77%, respectively. EDS mapping confirms the homogenous distribution of all elements (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ed-g). The presence of C and O is attributed to the RGO nanosheet (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ee and \u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ef). In contrast, the presence of the Co, and O elements is attributed to the CoO nanoparticles (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ef and \u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eg).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eXRD analysis was performed to explore the structural and crystalline characteristics of the RGO and RGOCoO hybrid. In the XRD patterns, Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e. illustrates the peak at 26.5\u0026deg; corresponding to the (002) crystal plane in RGO. The XRD analysis of the RGOCoO hybrid reveals relatively weak diffraction peaks, suggesting the crystallized nature of CoO. The peaks observed at 33.31\u0026deg;, 42.20\u0026deg;, and 59.24\u0026deg; correspond to the (110), (200), and (220) planes, respectively, following the standard cubic structure of CoO (JCPDS No. 43-1004)\u003csup\u003e51\u003c/sup\u003e. Furthermore, the presence of RGO in the synthesized hybrid is confirmed by the peak at 26.50\u0026deg;, corresponding to the (002) plane.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe utilization of FTIR Spectroscopy is pivotal for the development of the composites and hybrid to identify chemical bonds. Figure\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e illustrates the FTIR spectra showcasing IR bands for RGO and RGOCoO. The broad peak observed at 3434 cm⁻\u0026sup1; in RGO can be ascribed to the stretching vibration of hydroxyl groups. The spectral features between 2840\u0026ndash;2940 cm⁻\u0026sup1; correspond to the C\u0026ndash;H alkyl groups. Additionally, distinct IR bands at 1638 cm⁻\u0026sup1;, and 1577 cm⁻\u0026sup1; are associated with the carboxylic acid stretching vibrations of C\u0026thinsp;=\u0026thinsp;O, and the alkenes stretching vibration of the C\u0026thinsp;=\u0026thinsp;C bond, respectively. Moreover, the peaks at 1168 cm⁻\u0026sup1; and 1115 cm⁻\u0026sup1; correspond to OH deformation and bending vibration, epoxy stretching of C-O-C, and alkoxy stretching of C-O, respectively. The FTIR spectrum of the RGOCoO hybrid reveals the vibrations of RGO and the attenuation of the hydroxyl group's broadband\u003csup\u003e52\u003c/sup\u003e. The spectrum of the RGOCoO hybrid manifests two distinct and intense peaks at 1568 cm⁻\u0026sup1;, 661 cm⁻\u0026sup1; and 610 cm⁻\u0026sup1;, confirming the structure of CoO and the successful synthesis of the RGOCoO hybrid\u003csup\u003e53\u003c/sup\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe structural properties of the surfaces, such as specific surface area, pore size distribution, and N\u003csub\u003e2\u003c/sub\u003e adsorption-desorption isotherms, are elucidated through BET analysis, as depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea and b. A distinct hysteresis loop in the 0.4\u0026thinsp;\u0026minus;\u0026thinsp;1.0 P/P\u003csub\u003e0\u003c/sub\u003e range, indicating the N\u003csub\u003e2\u003c/sub\u003e adsorption-desorption isotherm of the electrode materials, closely resembling IV type with an H\u003csub\u003e3\u003c/sub\u003e hysteresis loop (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea). This observation indicates that the electrode materials possess a mesoporous structure. The RGOCoO shows a higher BET specific surface area of 59.59 m\u003csup\u003e2\u003c/sup\u003eg\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, accompanied by a pore volume measuring 13.69 cm\u003csup\u003e3\u003c/sup\u003e(STP) g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e compared to RGO with a specific surface area of 39.37, and a pore volume measuring 9.04 cm\u003csup\u003e3\u003c/sup\u003e(STP) g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. Additionally, in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb, the Barrett-Joyner-Halenda (BJH) plot reveals an average pore diameter of 4.60 nm for the produced RGOCoO and 7.82 nm for RGO composites, affirming the presence of mesoporous in RGOCoO. The combination of a high BET surface area and porous characteristics enhances the reaction area, facilitating improved electrolyte penetration and efficient transport of electrons and ions within the electrode matrix, ultimately leading to enhanced supercapacitive performance attributed to the synergistic properties of CoRGO \u003csup\u003e54\u003c/sup\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe straightforward fabrication process and synergistic properties position the RGOCoO hybrid as a promising candidate for applications in energy storage systems. To investigate the electrochemical performance of the RGOCoO electrodes, cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD) analyses were conducted in a 6 M KOH solution within a potential window of -0.1 to 0.45 V. The CV profiles of the RGOCoO and foam nickel were recorded at the scanning rate of 5 mV s⁻\u0026sup1;, illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ea. The CV curve of RGOCoO exhibits a significantly larger area compared to that of foam nickel, indicating the negligible impact of foam nickel on capacitance. Figure\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003eb displays the CV curves of the RGOCoO at various scan rates ranging from 5 to 80 mV s⁻\u0026sup1;. The nearly rectangular CV shapes suggest excellent capacitive behavior of the RGOCoO hybrid, with asymmetry likely stemming from the combination of double-layer capacitance (EDLC) from RGO and pseudocapacitance characteristics from the redox reaction of CoO. The emergence of a pair of subtle redox in the CV profiles of the hybrid is attributed to the following chemical reactions.\u003c/p\u003e \u003cp\u003eCoO\u0026thinsp;+\u0026thinsp;OH\u003csup\u003e\u0026minus;\u003c/sup\u003e \u0026harr; CoOOH\u0026thinsp;+\u0026thinsp;e\u003csup\u003e\u0026minus;\u003c/sup\u003e (\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e)\u003c/p\u003e \u003cp\u003eCoOOH\u0026thinsp;+\u0026thinsp;OH\u003csup\u003e\u0026minus;\u003c/sup\u003e \u0026harr; CoO\u003csub\u003e2\u003c/sub\u003e\u0026thinsp;+\u0026thinsp;H\u003csub\u003e2\u003c/sub\u003eO\u0026thinsp;+\u0026thinsp;e\u003csup\u003e\u0026minus;\u003c/sup\u003e (\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e)\u003c/p\u003e \u003cp\u003eGCD measurements of the RGOCoO were conducted at different current densities, as depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ec, with specific capacitances calculated from the corresponding discharge profiles. The RGOCoO hybrid demonstrates good capacitive performance, as illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ed, yielding specific capacitances of 132.3 mF cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e at 2 mF cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e. As the current density decreased, the capacitance values showed a notable increase. The reduction in specific capacitance as the current density increases can be elucidated as follows: The extended interaction duration between electrolyte ions and the RGOCoO electrode under low current density enables the accumulation of a significant charge quantity within the electrode, resulting in a high specific capacitance; and conversely, under high current density, the period of interaction between the electrolyte ions and the electrode is restricted. Consequently, a decreased specific capacitance is observed at higher current densities\u003csup\u003e32,55\u003c/sup\u003e. The cycling stability of the RGOCoO electrodes was assessed through charge/discharge cycling at a current density of 9 A cm⁻\u003csup\u003e2\u003c/sup\u003e. After 7000 cycles, as exhibited in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ee, the capacitance retention of the RGOCoO hybrid remains as high as 95.91%, indicating remarkable electrochemical stability.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe investigation of capacitive elements and charge transfer kinetics of the RGOCoO electrode was conducted using EIS, performed in a 6 M KOH solution across the frequency range of 10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e to 10\u003csup\u003e5\u003c/sup\u003e Hz. The EIS spectra of RGOCoO in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003ea display a linear trend with slight curvature in the higher frequency region, reflecting lower charge-transfer resistance and enhanced conductivity based on the Nyquist plot analysis. This improved performance can be attributed to the crumpled RGO sheets and the uniform dispersion of CoO spheres\u003csup\u003e56\u003c/sup\u003e. In the Bode plot illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003eb, the magnitude of total impedance |Z| decreased as the frequency increased. The resistive impedance shows minimal dependence on the frequency at 10 Hz and beyond. Figure\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003ec illustrates the correlation between the phase angle and frequency, indicating the notable capacitance effect at lower frequencies (54.32\u0026deg;). The relaxation time constant (τ) required to discharge more than 50% of the total energy at an angle of approximately 45\u0026deg; is the minimum discharge time\u003csup\u003e57\u003c/sup\u003e.\u003cdiv id=\"Equ2\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ2\" name=\"EquationSource\"\u003e\n$$\\tau =\\frac{1}{2\\pi {f}^{*}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e4\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eHere, specific frequency f* corresponding to a phase angle of 45\u0026deg; equates to a time constant of τ\u0026thinsp;=\u0026thinsp;0.53 s. This frequency marks the equilibrium point where the resistive and capacitive impedance components balance, leading to a shift towards a more resistive behavior in the supercapacitor at frequencies exceeding f*. This short time constant indicates a strong rate capability of the fabricated electrode material. In the AC response, the capacitor enters a complex domain that includes a real component C\u0026prime;(ω) and an imaginary component C\u0026Prime;(ω)\u003cdiv id=\"Equ3\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ3\" name=\"EquationSource\"\u003e\n$$C\\left(\\omega \\right)={C}^{{\\prime }}\\left(\\omega \\right)+iC{\\prime }{\\prime }\\left(\\omega \\right)$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e5\u003c/div\u003e\u003c/div\u003e\u003cdiv id=\"Equ4\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ4\" name=\"EquationSource\"\u003e\n$$C{\\prime }\\left(\\omega \\right)=\\frac{-{z}^{\u0026quot;}\\left(\\omega \\right)}{\\omega \\times {\\left|Z\\left(\\omega \\right)\\right|}^{2}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e6\u003c/div\u003e\u003c/div\u003e\u003cdiv id=\"Equ5\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ5\" name=\"EquationSource\"\u003e\n$$C{\\prime }{\\prime }\\left(\\omega \\right)=\\frac{-{Z}^{{\\prime }}\\left(\\omega \\right)}{\\omega \\times {\\left|Z\\left(f\\right)\\right|}^{2}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e7\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003ewhere the total capacitance is denoted by |C(ω)|\u0026sup2; and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\omega =2\\pi f\\)\u003c/span\u003e\u003c/span\u003e. The total impedance magnitude, real part (Z'), and imaginary part (Z'') are denoted as |Z|, Z', and Z'', respectively. In Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003ed, the plot illustrates the relationship between real capacitance and real resistance, defining the charging behavior of the electrode. The activated material displayed an increase in resistance as capacitance increased. This phenomenon can be attributed to the penetration of the AC signal into pores of different sizes, resulting in the stabilization of capacitance levels. The imaginary and real components of capacitance are depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003ee and f, illustrating a decrease in capacitance with increasing frequency. There is a decreasing trend from a frequency of 0.01 Hz to 10 Hz, while the trend remains constant at frequencies higher than 10 Hz. Ideally, pure capacitance possesses no real part as it contributes solely to power, while the imaginary part of capacitance, C\u0026Prime;(ω), accounts for energy dissipation in an irreversible process.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe enhanced electrochemical properties of the RGOCoO electrode can be attributed to several factors, including the notably larger specific surface area of the RGOCoO hybrid, which plays a crucial role in increasing the electron transfer rate. The specific structure of the hybrid facilitates electrolyte access to the electrochemical sites, resulting in shorter diffusion paths for adsorbing ions. Moreover, the crumpled RGO with numerous wrinkles and folds can promote high electronic conductivity and provide more reactive sites. These characteristics accelerate ion and charge transport during the charge/discharge process, improving cycle life stability\u003csup\u003e56\u003c/sup\u003e.\u003c/p\u003e"},{"header":"Conclusion","content":"\u003cp\u003eTo summarize, a facile one-step approach has been introduced for the to fabricate of the RGOCoO electrode, resulting in the crumpled RGO sheets being non-uniformly distributed alongside CoO spheres. Hybrid electrode RGOCoO, offer the advantage that they serve as electrodes independently, without requiring additional active components like binders or conductive additives. The CoO, when combined with the crumpled RGO, offers synergistic characteristics by skillfully blending pseudocapacitive and EDLC-type materials. Expanding the external surface area enhances the effective interaction with ions in the electrolyte, and optimizing the pore size to match the ion size maximizes capacitance. This configuration enhances the electrical conductivity of the RGOCoO hybrid, making it suitable for use as an electrode. The optimized RGOCoO electrodes exhibited a notable specific capacitance of 132.3 mF cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e and a remarkable capacitance retention of 95.91% after 7000 cycles. The rapid energy release indicated by the relaxation time of 0.53 s highlights the exceptional rate performance of the RGOCoO based supercapacitor, demonstrating the efficacy of this nanostructured material for high-performance energy storage applications.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e \u003ch2\u003eSupporting Information\u003c/h2\u003e \u003cp\u003eAn accompanying supplementary document has been provided for this manuscript, which includes supplementary EDS analysis.\u003c/p\u003e \u003c/p\u003e\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eS. M.Q.: Research and experiments, main researcher, writing manuscript (https://orcid.org/0000-0002-5419-9209). M.R.Z.M.:Project lead, conceptualization, validation, reviewing, and editing (https://orcid.org/0000-0002-8802-807X). A.M.: Conceptualization, validation, reviewing, and editing (https://orcid.org/0000-0001-5490-3350).\u003c/p\u003e\u003ch2\u003eAcknowledgement\u003c/h2\u003e\u003cp\u003eWe extend our sincere gratitude to our esteemed colleagues at the Materials and Nanotechnology Research Laboratory (MNT Lab). Additionally, we would like to thank the Iran Fuel Conservation Company (IFCO) for their valuable assistance. We sincerely acknowledge the support of the Iran University of Science and Technology (IUST) and express our gratitude to their Central Laboratory, Physics Laboratory Services, and Chemistry Laboratory Services for their invaluable contributions to this research endeavor. We are also thankful to the Iran High-Tech Laboratory Network (Labsnet) for providing the necessary research facilities.\u003c/p\u003e\u003ch2\u003eData Availability\u003c/h2\u003e\u003cp\u003eAll data generated or analysed during this study are included in this published article [and its supplementary information files].\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eDutta, A., Mitra, S., Basak, M. \u0026amp; Banerjee, T. A comprehensive review on batteries and supercapacitors: Development and challenges since their inception. Energy Storage 5, e339 (2023).\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eSalgado-Pizarro, R., Calder\u0026oacute;n, A., Svobodova-Sedlackova, A., Fern\u0026aacute;ndez, A. I. \u0026amp; Barreneche, C. The relevance of thermochemical energy storage in the last two decades: The analysis of research evolution. J. 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Mater. 22, 4501\u0026ndash;4510 (2012).\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"scientific-reports","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scirep","sideBox":"Learn more about [Scientific Reports](http://www.nature.com/srep/)","snPcode":"","submissionUrl":"","title":"Scientific Reports","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Scientific Reports","inReviewEnabled":true,"inReviewRevisionsEnabled":true},"keywords":"Graphene Oxide, Hybrid, Cobalt Oxide, Supercapacitor, Inexpensive, Facile Synthesis, Relaxation Time","lastPublishedDoi":"10.21203/rs.3.rs-4414730/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-4414730/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThe increasing need for electrode materials exhibiting improved performance to meet the requirements of supercapacitors is on the rise. Hybrid electrodes, which combine reduced graphene (RGO) oxide with transition metal-based oxides such as cobalt oxide (CoO), have emerged as promising materials due to their impressive specific capacitance and cost-effectiveness, attributed to their synergistic properties. In the present study, a binder-free RGOCoO composite electrode was synthesized using a facile, fast, and simple one-step co-precipitation method. This was done to improve stability for supercapacitor applications. The synthesized composite materials underwent comprehensive characterization utilizing various surface analytical techniques, including X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), field-emission scanning electron microscopy (FE-SEM), fourier-transform infrared spectroscopy (FTIR), and Brunauer\u0026ndash;Emmett\u0026ndash;Teller (BET) analysis. Electrochemical measurements of the fabricated hybrid revealed at current density of 2 A cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e a specific capacitance of 132.3 mF cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e, with an impressive 95.91% retention of capacitance after 7000 cycles. The results from electrochemical impedance spectroscopy (EIS) highlighted a meager low relaxation time constant of 0.53 s for the electrode. The reason behind this can be linked to the synergistic interactions, and minimal charge transfer resistance exhibited by the porous electrode without binders. The innovative simple synthesis of a binder-free RGOCoO composite electrode represents a significant advancement in the development of high-efficiency supercapacitors for diverse large-scale applications.\u003c/p\u003e","manuscriptTitle":"A Simple Method for Fabrication of Hybrid Electrodes of Supercapacitors","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-06-03 14:03:15","doi":"10.21203/rs.3.rs-4414730/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2024-10-16T15:36:28+00:00","index":"","fulltext":""},{"type":"reviewerAgreed","content":"269807096073592896082341427103755055441","date":"2024-08-28T06:31:47+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-08-28T06:01:34+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"89645399014589573167189325007580526907","date":"2024-08-26T10:07:56+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-06-05T05:48:25+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"263706283056500092568379910925003732094","date":"2024-05-19T12:51:32+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"312313132341185453377703927899596708602","date":"2024-05-19T09:46:15+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2024-05-19T07:14:22+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2024-05-19T06:58:58+00:00","index":"","fulltext":""},{"type":"editorInvited","content":"","date":"2024-05-19T06:33:41+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2024-05-17T05:19:36+00:00","index":"","fulltext":""},{"type":"submitted","content":"Scientific Reports","date":"2024-05-13T17:39:03+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"scientific-reports","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scirep","sideBox":"Learn more about [Scientific Reports](http://www.nature.com/srep/)","snPcode":"","submissionUrl":"","title":"Scientific Reports","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Scientific Reports","inReviewEnabled":true,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"de37945d-55eb-41bd-a6ca-e3c067b1dc39","owner":[],"postedDate":"June 3rd, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[{"id":32292363,"name":"Physical sciences/Materials science/Materials for devices"},{"id":32292364,"name":"Physical sciences/Chemistry/Electrochemistry"}],"tags":[],"updatedAt":"2024-11-25T16:02:36+00:00","versionOfRecord":{"articleIdentity":"rs-4414730","link":"https://doi.org/10.1038/s41598-024-80243-2","journal":{"identity":"scientific-reports","isVorOnly":false,"title":"Scientific Reports"},"publishedOn":"2024-11-24 15:57:44","publishedOnDateReadable":"November 24th, 2024"},"versionCreatedAt":"2024-06-03 14:03:15","video":"","vorDoi":"10.1038/s41598-024-80243-2","vorDoiUrl":"https://doi.org/10.1038/s41598-024-80243-2","workflowStages":[]},"version":"v1","identity":"rs-4414730","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-4414730","identity":"rs-4414730","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}