Synthesis and Electrochemical Performance of ZnO:MnO:VO Ternary Metal Oxide Nanocomposite for Supercapacitor Applications

Synthesis and Electrochemical Performance of ZnO:MnO:VO Ternary Metal Oxide Nanocomposite for Supercapacitor Applications | 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 Research Article Synthesis and Electrochemical Performance of ZnO:MnO:VO Ternary Metal Oxide Nanocomposite for Supercapacitor Applications Rekha Kumari, Yogesh Kumar, Vivek Kumar Shukla This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6304051/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract This investigation describes both the synthesis process and detailed inspection of ZnO:MnO:VO nanocomposites which were made through hydrothermal processing and subsequent heating treatment. X-ray diffraction results showed that the prepared nanocomposite structure primarily contained the FCC phase of MnO and small amounts of Wurtzite ZnO and Orthorhombic VO phases. The nanocomposite contains tiny crystalline grains rabged from 1.50 to 3.71 nm, as determined through the Debye-Scherrer formula. The characteristic FTIR vibrational modes from metal-oxygen (M–O) bonds validated the composite formation in the analysis. The Scanning Electron Microscope showed rod-shaped components with lengths from 1 µm to 10 µm and Energy Dispersive X-ray Spectroscopy demonstrated that all four atomic elements of Zn, Mn and V and O existed evenly throughout the composite structure. The structural analysis showed strong crystalline content and complete phase purity because no additional impurities were present. The electrochemical assessment of the ZnO:MnO:VO nanocomposite took place through CV and GCD and EIS testing in 1M KOH aqueous electrolyte. The specific capacitance by CV and GCD analysis were found 232.11 Fg⁻¹ and 222.75 Fg⁻¹ respectively. The structural and morphological properties of ZnO:MnO:VO nanocomposite are suitable for supercapacitor applications and finds high capacitive devices. Supercapacitors ZnO:MnO:VO Ternary Metal Oxide Hydrothermal synthesis XRD SEM EDX FTIR TEM CV GCD and EIS Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Introduction Advanced research on supercapacitor electrode materials has been intensified because industries worldwide need better and greener energy storage techniques. Supercapacitors demonstrate their importance as fundamental parts in renewable energy systems and portable electronics along with hybrid electric vehicles because they have excellent characteristics such as rapid charge-discharge rates and up to 10 kW/kg power density along with cycle stability exceeding 1,000,000 cycles[ 1 ]. Superconductors have a small energy density of 5 to 10 Wh/kg that restricts their broader usage compared to batteries[ 2 ]. The solution to this challenge demands new strategies that will enhance the specific capacitance and extend the potential window range of electrode materials. Superior energy storage functions of supercapacitors has been developed through the incorporation of transition metal oxides like MnO₂, ZnO and VOₓ. The pseudocapacitive applications of MnO₂ benefit from abundant studies because of its high theoretical specific capacitance value at 1370 F/g alongside economical prices [ 3 ]. The theoretical capacitance of ZnO stands high at ~ 750 F/g while its environmental compatibility serves as an advantage for its use in energy storage devices[ 4 ]. Among various advantages of vanadium oxides (VOₓ) lie the capability to shift between V⁵⁺ ↔ V³⁺ valence states which results in rapid charge transfer and high energy density up to ~ 400 Wh/kg[ 5 – 7 ]. These materials alone face implementation hurdles because of their inadequate electrical transmission and their poorly stable repeated charge-discharge cycles[ 8 , 9 ]. The development of composite materials through several integrated transition metal oxides creates synergistic characteristics to address the existing challenges[ 10 – 15 ]. Research has shown that hydrothermal reaction techniques enable the synthesis of Mn-Cu-Ni composites which perform well in terms of specific capacitance alongside cycling stability verification[ 16 ]. Trimetallic fluorides which contain Ni-Co-Zn have demonstrated outstanding achievement with their high specific capacitance values and extended cyclic durability[ 17 ]. The research confirms that combined multi-component systems have the ability to improve charge storage alongside cyclic performance durability[ 18 ]. The production and characterization of ZnO:MnO:VO (1:1:1 molar wt.) nanocomposite powders are described in detail based on hydrothermal processing then thermal treatment steps. The nanocomposite contains MnO as a main redox capacity contributor with ZnO serving as an environmentally friendly substance and VO providing multiple charge storage characteristics. Different techniques such as X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy and Fourier-transform infrared spectroscopy and transmission electron microscopy were used to characterize the synthesized materials. System performance measurements used cyclic voltammetry as well as galvanostatic charge-discharge tests and electrochemical impedance spectroscopy. Evaluation outcomes indicate that the ZnO:MnO:VO combination exists as a promising material for supercapacitor applications using advanced storage technologies for upcoming energy solutions. Experimental Section Synthesis of material The synthesis of ZnO:MnO:VO (1:1:1) nanocomposite powder started with preparing 50 mL of 0.1 M solutions by dissolving ammonium metavanadate (NH₄VO₃, 2.18 g) and manganese acetate tetrahydrate [(CH₃COO)₂Mn·4H₂O, 2.44 g] together with zinc acetate dihydrate [Zn(CH₃COO)₂·2H₂O, 1.16 g] in distilled water. The mixture of precursors received 5 mL of Polyethylene glycol (PEG) which later underwent 30 minutes of stirring with a magnet at room temperature to achieve mixture uniformity. The solution received a transfer into a 250 mL Teflon-lined stainless steel autoclave for hydrothermal treatment at 100°C over a period of 16 hours. The precipitate was separated through centrifugation at 5000 rpm for 5 minutes and this process was performed several times (4 to 5 repetitions) before washing with ethanol and distilled water until pH became neutral. The ZnO:MnO:VO nanocomposites were produced by subjecting the product to six hours of calcination at 300°C under air conditions. Material characterization The analysis of synthesized samples through X-ray diffractometry (Panalytical Xpert Pro) utilized CuKα radiation (k = 1.54 Å) for a 2θ Bragg angle range from 10° to 80° to determine both crystallinity and phase composition. The Perkin Elmer instrument was used for FTIR spectroscopy to detect functional groups that exist in the material. EDS from Bruker analyzed the elemental content of the material while SEM from GEOL M-MUJ served to study the high magnification surface topography of the material. TEM analysis using Tachnai 200 Model generated images that showed clear grain boundaries while detecting thin dislocations occurring inside the grains. The EmStat4S electrochemical workstation operated GCD and CV and EIS tests on the materials. The EDLCs required CV evaluation through multiple scan rates between 0 and 0.8 V utilizing values of 3, 5, and 7 mV s − 1. At different current densities between 2 and 5 A g − 1 and within the potential range of 0–0.8 V the GCD experiment occurred. EIS analysis spanned frequencies from 0.01 Hz to 100 kHz. Fabrication of Electrodes To make the working electrode, 80% of the Zn-Mn-V oxide nanocomposite was mixed with 10% polyvinylidene fluoride (PVDF) and 10% acetylene black (AB). This mixture was then turned into a paste using N-methyl-2-pyrrolidone (NMP) as the solvent.Then, the prepared paste was evenly spread over a 1 × 1 cm² area of the graphite sheet. The coated electrode was dried in the oven at 80°C for 12 hours to make sure everything sticks properly and the solvent evaporates. Results and Discussion X-ray Diffraction (XRD) X-ray diffraction (XRD) was utilized to investigate the crystalline structure and phase composition of the synthesized ZnO:MnO:VO. XRD measurements were performed using a Panalytical with Cu Kα radiation (λ = 1.54060 Å) over a 2θ range from 10° to 80°. The XRD pattern exhibited distinct peaks at 2θ values of 18.75, 24.23, 30.40, 36.28, 38.18, 40.41, 52.75, 53.68, 64.90, which were indexed to the (100), (110), (111), (200), (002), (211), (220), (311), (222) respectively. The MnO (FCC) major peaks are identified as (111), (200), (220), (311) and confirmed by JCPDS No. 75–0626[ 19 ], ZnO (Wurtzite, Hexagonal) major peaks are found (100), (101), (102) confirmed by JCPDS No. 36-1451[ 20 ] and VO Orthorhombic at (110 ) JCPDS 41-1426[ 21 ]. To assess the lattice parameters, the diffraction angles for the prominent peaks were used to calculate the d-spacing values using Bragg’s law. The crystallite size of the synthesized ZnO:MnO:VO nanocomposite was calculated using the Scherrer equation: $$\:D=\frac{\text{K}{\lambda\:}}{{\beta\:}\text{c}\text{o}\text{s}{\theta\:}}$$ where D is the crystallite size, K is the shape factor (0.9), λ is the X-ray wavelength (0.154 nm), β is the FWHM (full width at half maximum), and θ is the Bragg angle. The calculated crystallite sizes ranged from 1.50 nm to 3.71 nm, indicating the formation of fine crystalline grains. Specific values include 3.57 nm at 18.7572°, 1.50 nm at 24.2304°, and 3.71 nm at 36.2807°, with other peaks corresponding to crystallite sizes between these ranges[ 22 ]. The absence of additional peaks associated with impurity phases confirms the high phase purity of the material. The XRD results demonstrate the successful synthesis of the ZnO:MnO:VO nanocomposite with well-defined crystalline characteristics, providing valuable insights into its structural properties and potential electrochemical applications. Scanning Electron Microscopy (SEM) The SEM analysis provides detailed insights into the surface morphology of the sample. Figure 2 , displays the SEM images of the ZnO:MnO:VO nanocomposite at different magnifications, revealing a well-defined nanorod morphology[ 23 ]. In Fig. 2 (a) at 30,000x magnification, the nanorods exhibit diameters ranging from 80–120 nm and lengths of approximately 500–700 nm, with smooth surfaces and sharp edges, indicating uniform crystal growth. Figure 2 (b) at 10,000x magnification shows the agglomeration of nanorods into hierarchical structures, which enhances the surface area and may improve electrochemical performance. Figure 2 (c) at 5,000x magnification further highlights the interconnected nanorods, suggesting homogeneous dispersion across the composite[ 24 ]. At 2,000x magnification in Fig. 2 (d), a broader field of view confirms the uniform distribution of nanorods throughout the sample[ 25 ]. The absence of significant structural defects across all scales indicates the successful synthesis of a highly crystalline ZnO:MnO:VO nanocomposite, which is suitable for supercapacitor and energy storage applications. Energy-Dispersive X-ray (EDX) The EDX analysis of the ZnO:MnO:VO nanocomposite confirms the presence of oxygen (O), vanadium (V), manganese (Mn), and zinc (Zn), which are the primary constituents of the composite. The quantitative analysis reveals that vanadium is the most dominant element, accounting for 41.0 wt.%, followed by manganese (34.4 wt.%), oxygen (15.6 wt.%), and zinc (9.0 wt.%). The detected elemental ratios align closely with the expected composition, confirming the successful incorporation of these metal oxides during the hydrothermal synthesis and subsequent calcination[ 26 ]. The absence of any additional peaks in the EDX spectrum indicates high purity of the synthesized composite without any contamination or unwanted secondary phases. The elemental mapping images further illustrate the spatial distribution of each element across the sample surface. The oxygen (O) map (Figure a) reveals a homogeneous distribution, confirming the presence of metal oxides uniformly dispersed throughout the nanocomposite matrix[ 27 ]. The zinc (Zn) map (Figure b) shows a well-scattered, consistent distribution, supporting the successful incorporation of the ZnO phase[ 28 , 29 ]. The vanadium (V) map (Figure c) displays a uniform spread of vanadium, confirming its successful incorporation and even dispersion within the composite[ 30 ]. Similarly, the manganese (Mn) map (Figure d) indicates an even and widespread presence of manganese, which aligns with the significant contribution of the MnO phase identified by XRD[ 31 ]. The consistent and uniform distribution of all these elements suggests homogeneity within the nanocomposite, which is essential for achieving superior electrochemical performance[ 32 ]. Transition Electron Microscope (TEM) In Fig. 4 (a) TEM imaging reveals the presence of well-defined nanorod with lengths 585 nm and diameter is 65 nm, confirming a rod-like morphology. The nanorod length and width were calculated by ImageJ software. The Selected Area Electron Diffraction (SAED) pattern from the Transmission Electron Microscope (TEM) confirms a crystalline structure with distinct diffraction spots and concentric rings, indicating a polycrystalline nature in Fig. 4 (b)[ 33 ]. Image analysis identified eight prominent diffraction rings, with calculated d-spacing values of 0.118 nm, 0.081 nm, 0.063 nm, 0.057 nm, 0.050 nm, 0.044 nm, 0.040 nm, and 0.037 nm, derived using the provided scale of 5.00 1/nm[ 34 ]. The observed d-spacing values closely align with the face-centered cubic (FCC) structure, particularly the (111), (200), and (220) planes, which have characteristic d-spacings of 0.202 nm, 0.143 nm, and 0.117 nm, respectively. Additionally, the measured 0.118 nm corresponds to the (211) plane of the body-centered cubic (BCC) structure, which also includes 0.203 nm (110) and 0.144 nm (200). However, the data does not match the typical d-spacings of the hexagonal close-packed (HCP) structure, reinforcing the dominance of FCC and potential BCC phases. The crystallite size was calculated using the Debye-Scherrer equation from both the SAED and XRD patterns[ 35 ]. The TEM-SAED analysis yielded a crystallite size range of 2.10 nm to 4.05 nm, which slightly exceeds the XRD-based estimation of 1.50 nm to 3.71 nm, suggesting the presence of fine, highly crystalline grains. The SAED results align closely with X-ray Diffraction (XRD) findings, where reflections at 18.75°, 24.23°, 30.40°, and 36.28° correspond to the (111), (200), (220), and (311) planes of the MnO (FCC) phase, confirmed by JCPDS No. 75–0626. The SAED-derived d-spacings support the identification of the FCC structure and match the key reflections observed in XRD. The clear and uniform diffraction rings indicate a high degree of crystallinity with minimal structural defects.[ 36 , 37 ] Furthermore, comparison with crystallographic databases supports the presence of ZnO (Wurtzite, Hexagonal) and VO (Orthorhombic) phases, though their contributions are less pronounced in the SAED pattern. This comprehensive analysis confirms the successful synthesis of the ZnO:MnO:VO composite with high crystallinity and phase purity, as evidenced by the strong agreement between SAED and XRD results. FTIR The FTIR spectrum of the ZnO:MnO:VO nanocomposite provides insight into the functional groups and metal-oxygen bonding present in the material. The broad absorption band observed around 3350 cm⁻¹ corresponds to the O-H stretching vibration of hydroxyl groups, indicating the presence of residual moisture or surface-adsorbed water [ 38 ]. This is common in metal oxide nanomaterials due to their high surface area. The weak band near 1634 cm⁻¹ can be attributed to the H-O-H bending vibration, further confirming adsorbed water molecules[ 39 ]. The V–O stretching vibrations that give rise to a substantial peak reaching 816.42 cm⁻¹ indicate the presence of vanadium oxides (VOₓ) and V–O–M linkages which include zinc or manganese metals (M)st[ 40 ]. The qualitative analysis shows that the composite contains successfully incorporated vanadium units. A group of strong peaks located between 500–600 cm⁻¹ identifies the Zn–O and Mn–O stretching bonds indicating that zinc oxide (ZnO) and manganese oxide (MnO) phases have formed[ 41 , 42 ]. Research findings from mixed metal oxides demonstrate an agreement with current results which confirms the presence of all desired phases[ 43 ]. The FTIR analysis reveals no major organic peaks because the organic residues successfully removed throughout the calcination step. The nanocomposite ZnO:MnO:VO succeeds in its formation as confirmed through characteristic peaks which indicate strong metal-oxygen bonding[ 44 ]. The successful synthesis of well-defined ZnO:MnO:VO nanocomposite was validated through FTIR analysis which supplemented the XRD and TEM-SAED results. The extensive characterizations reveal all the necessary features for this material to demonstrate promising energy storage performance because strong metal-oxygen bonds combined with structural stability enhance electrochemical performance. Electrochemical Performance: Evaluation of ZnO:MnO:VO nanocomposite electrode electrochemical performance levels required electrochemical test execution. The aqueous electrolytes allow voltage operation between 0.8V because electrolysis occurs beyond this limit. The electrochemical testing process of ZnO:MnO:VO electrode based supercapacitors involved 1M KOH aqueous electrolyte solutions tested through − 0.4V to 0.4V potential. Compositional ratio of synthesis material, binder and conducting material and electrolytes was 80:10:10 employed to create electrodes for the assembly of device. The binder PVDF provide mechanical qualities to carbon particles, but they also contribute the electrode material's electric and ionic resistance, limiting the device's power capabilities, due to that reason conducting materials are used to compensate ionic and electric resistance [ 45 ]. Cyclic voltammetry (CV) A CV analysis was performed through various scan rates between 3 mVs⁻¹ to 7 mVs⁻¹ and a potential scope from − 0.4V to 0.4V. The capacitor typical curve appears in Fig. 6 . A perfect CV curve profile with symmetrical shapes adjacent to zero current appears on the ZnO:MnO:VO cells when the scan rate remains low indicating quick and reversible charge and discharge processes without redox reactions. Raising the scan rate does not alter the symmetrical appearance of the CV indicating the charging process maintains consistency with the discharging process. The size of the CV area grows bigger as the scan rate increases since faster scan rates result in greater ion concentration. This affects the device's performance. The energy storage capacity grows larger because the ions accelerate their movement within electrolyte pores[ 46 ]. The specific capacitance measurements from cyclic voltammetry reached 232.11, 195.41, and 178.42 Fg⁻¹ at the different scan rates between 3, 5, and 7 mVs⁻¹. The research data shows that specific capacitance diminishes when the scan rate grows higher. The electrode active sites are easier to reach by ions when scan rates remain low thus permitting better ion insertion. The measurement of higher capacitance occurs at scan rates that remain low. Galvanostatic charge-discharge (GCD) A near-symmetrical triangular shape represents the GCD curves of the supercapacitor constructed with ZnO:MnO:VO electrodes as per Fig. 7 . The capacitive behavior and operating efficiency of the supercapacitor appear excellent based on this result. The symmetric cells received specific capacitance calculation using a stated formula found in reference [ 47 ]. $$\:{C}_{s}=2\frac{I\varDelta\:T}{m\varDelta\:U}$$ 1 The measurement combines m for mass of one electrode with I as current and has two time intervals Δt and potential range ΔU. Figure 7 shows the GCD curves at different current densities (2, 3, 4, and 5 A/g) at 0.8V. The calculated specific capacitances were 222.75 F/g, 213.37 F/g, 197 F/g, and 178.75 F/g for the corresponding current densities of 2, 3, 4, and 5 A/g. Electrochemical Impedance Spectroscopy (EIS) To understand the mobility or limitation of ion transport in porous architecture of ZnO:MnO:VO, EIS was also performed. Figure 8 depicts the Nyquist fitted plots for fabricated of ZnO:MnO:VO electrode device with in a frequency range of 0.01 Hz to 100 KHz to determine the charge transfer process. The straight line in the Nyquist spectra indicates a low charge transfer resistance of electrode material's with excellent pseudocapacitive properties [ 46 , 47 ]. The measurement technique incorporates all resistive elements into the electrolyte resistance (Rs). Electrolyte resistance and charge transfer resistance show low levels in the intervals of low frequency according to the Nyquist plot data. Studies have shown that ZnO:MnO:VO develops electrolyte resistances (Rs) equal to 11.4Ω. Nanoparticles of ZnO:MnO:VO exhibit electrodes with low resistance which offer simple pathways for charge intercalation and de-intercalation between the electrode and electrolyte according to ESI results. Zsimpwin 3.20 software enabled the fitting process which established R1(C1R2)(Q1R3)(C2R4) as the equivalent Randles circuit for the cells. Few of the various cell resistances have been named R1, R2, R3, R4 respectively. The equivalent Randles circuit for the cell uses R2 as grain resistance while R1 represents Ohmic contact resistance and R4 and R3 stand for sample–electrode interface and grain boundary resistance. The sub-circuit Q1R3 contains a constant phase element Q1 while C1 along with C2 represent parallel capacitances within C1R2 and C2R4 components respectively. Grain resistance (R2) becomes lower as the frequency increases yet the interface resistance (R4) and grain boundary resistance (R2) show a rising pattern according to frequency changes. Conclusion The ZnO:MnO:VO nanocomposite is successfully synthesized through hydrothermal processing followed by calcination which contains MnO (FCC), ZnO (Wurtzite, Hexagonal) and VO (Orthorhombic). The XRD results showed highly crystalline structures with crystallite dimensions between 1.50 nm to 3.71 nm and the FTIR patterns matched with metal-oxygen functional bonds. SEM showed that nanocomposite materials presented rod-shaped features extending from 1 µm to 10 µm while elemental distribution across the structure was verified through EDX examination. The structural stability together with purity and dimensional control of the composite indicates its suitability for use in supercapacitors and additional energy storage systems. The electrochemical performance of the ZnO:MnO:VO nanocomposite was evaluated using cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS) in 1M KOH aqueous electrolyte. The specific capacitance found by CV and GCD analysis was 232.11 Fg⁻¹ and 222.75 Fg⁻¹ respectively. Hence, the structural and morphological properties of ZnO:MnO:VO nanocomposite are suitable for high capacitive supercapacitor. Declarations Competing Interests The authors declare no competing interests. Funding There is no financial support was received for the research, authorship or publication of this manuscript. Author Contribution CRediT authorship contribution statementRekha Kumari : Writing – original draft, Methodology, Investigation, Formal analysis. Vivek Kumar Shukla: Writing – original draft, review& SupervisionYogesh Kumar: Writing – review & editing Acknowledgement One of the authors Rekha Kumari acknowledge the University Grant Commission (UGC), India for providing her financial support through JRF fellowship in this duration and Dr. Anurag Tyagi for scientific discussions. References Dissanayake K, Kularatna-Abeywardana D (2024) A review of supercapacitors: Materials, technology, challenges, and renewable energy applications. 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Materials Today Physics 38:101252. https://doi.org/10.1016/j.mtphys.2023.101252 Alamdari S, Sasani Ghamsari M, Lee C, et al (2020) Preparation and Characterization of Zinc Oxide Nanoparticles Using Leaf Extract of Sambucus ebulus. Applied Sciences 10:3620. https://doi.org/10.3390/app10103620 Albouchi W, Meftah M, Ben Haj Amara A, Oueslati W (2023) Effect of reactant ratio and nanofillers type on the microstructural properties, porosity fluctuations and heavy metal removal ability of chitosan-clay hybrid materials. Applied Surface Science Advances 13:100387. https://doi.org/10.1016/j.apsadv.2023.100387 Shafeeq KM, Athira VP, Kishor CHR, Aneesh PM (2020) Structural and optical properties of V2O5 nanostructures grown by thermal decomposition technique. Appl Phys A 126:586. https://doi.org/10.1007/s00339-020-03770-5 Aghmasheh M, Rezvani MA, Jafarian V, Ardeshiri HH (2023) Synthesis and Characterization of a New Nanocatalyst Based on Keggin-Type Polyoxovanadate/Nickel-Zinc Oxide, PV14/NiZn2O4, as a Potential Material for Deep Oxidative Desulfurization of Fuels. Energy Fuels 37:9474–9486. https://doi.org/10.1021/acs.energyfuels.3c01082 Oluwasogo DA, Varangane S, Prabhu YT, et al (2023) Biosynthetic modulation of carbon-doped ZnO for rapid photocatalytic endocrine disruptive remediation and hydrogen evolution. Journal of Cleaner Production 394:136393. https://doi.org/10.1016/j.jclepro.2023.136393 Solution Combustion Synthesis of Nanoscale Materials | Chemical Reviews. https://pubs.acs.org/doi/10.1021/acs.chemrev.6b00279 . Accessed 22 Mar 2025 Raizada P, Sudhaik A, Singh P (2019) Photocatalytic water decontamination using graphene and ZnO coupled photocatalysts: A review. Materials Science for Energy Technologies 2:509–525. https://doi.org/10.1016/j.mset.2019.04.007 López-Chavéz R, Gallegos A (2013) The Effect of Binder in Electrode Materials for Capacitance Improvement and EDLC Binder-free Cell Design. Journal of New Materials for Electrochemical Systems 16:197–202. https://doi.org/10.14447/jnmes.v16i3.17 Kumar Y, Chopra S, Gupta A, et al (2020) Low temperature synthesis of MnO2 nanostructures for supercapacitor application. Materials Science for Energy Technologies 3:566–574. https://doi.org/10.1016/j.mset.2020.06.002 Uke SJ, Chaudhari GN, Bodade AnjaliB, Mardikar SP (2020) Morphology dependant electrochemical performance of hydrothermally synthesized NiCo2O4 nanomorphs. Materials Science for Energy Technologies 3:289–298. https://doi.org/10.1016/j.mset.2019.11.004 Additional Declarations No competing interests reported. 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Kumar","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA4ElEQVRIiWNgGAWjYDACHgYGZih1AEhLyJCihS0BpIWHaC0glgGUTwAYnDnA9riwrU6Gv//M51c3aix4GNgPH92AV8vZBnbjmW2HeSRu5G6zzjkGdBhPWtoNvFrOM7BJ87Yd4DGQ4N1mnMMG1CLBY0aMljoeA/4zz4xz/hGj5WwDSAsz0O85zI9z24jQInnmYLsxzzmQX9LMmHP7JHjYCPmF70zyscc8ZXX2/P2HH3/O+VYnx89++BheLQoHGNsYGNnAbDYJMIlPOQjIN4DU/AGzmT8QUj0KRsEoGAUjEwAAO5NBcV7hVyoAAAAASUVORK5CYII=","orcid":"","institution":"Government College","correspondingAuthor":true,"prefix":"","firstName":"Yogesh","middleName":"","lastName":"Kumar","suffix":""},{"id":437221256,"identity":"eb0f49ec-dd2f-45f2-9b21-0abc8dd39535","order_by":2,"name":"Vivek Kumar Shukla","email":"","orcid":"","institution":"Gautam Buddha University","correspondingAuthor":false,"prefix":"","firstName":"Vivek","middleName":"Kumar","lastName":"Shukla","suffix":""}],"badges":[],"createdAt":"2025-03-25 13:08:53","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6304051/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6304051/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":79867852,"identity":"338ca587-6a89-4c53-af88-a2f8a9d4aaaf","added_by":"auto","created_at":"2025-04-03 19:47:09","extension":"jpg","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":159272,"visible":true,"origin":"","legend":"\u003cp\u003eX-ray diffraction of ZnO:MnO:VO.\u003c/p\u003e","description":"","filename":"1.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6304051/v1/7ba86f8727d93834fcc8c819.jpg"},{"id":79867609,"identity":"ed88ecc3-e04c-4ff5-955d-354ea3fddf2f","added_by":"auto","created_at":"2025-04-03 19:39:09","extension":"jpg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":65929,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of ZnO:MnO:VO: (a) at 30,000x, (b) at 10,000x \u0026nbsp;(c) at 5,000x and (d) at 2,000x.\u003c/p\u003e","description":"","filename":"2.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6304051/v1/f689c0af56ec847248b55cd4.jpg"},{"id":79867614,"identity":"290e79ee-2f4a-4842-9663-f0471973b9ed","added_by":"auto","created_at":"2025-04-03 19:39:09","extension":"jpg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":390569,"visible":true,"origin":"","legend":"\u003cp\u003eEDX analysis of ZnO:MnO:VO: (a) elemental mapping of material, oxygen (O), (b) Mn, (c) Zn ) (d) V (e) peak list with wt.% and at.%,\u003c/p\u003e","description":"","filename":"3.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6304051/v1/222223da13c5494fb8d28814.jpg"},{"id":79867853,"identity":"5c27463a-2379-4ad1-a466-bf50fb36ff67","added_by":"auto","created_at":"2025-04-03 19:47:09","extension":"jpg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":20843,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Represents the shape of nanorod and (b) SAED pattern of the ZnO:MnO:VO composite obtained from TEM.\u003c/p\u003e","description":"","filename":"4.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6304051/v1/c88497b88c7b4f475be7511b.jpg"},{"id":79867612,"identity":"0ff6b19d-bcf8-4f1d-8a92-6bf1f1a2de0a","added_by":"auto","created_at":"2025-04-03 19:39:09","extension":"jpg","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":25938,"visible":true,"origin":"","legend":"\u003cp\u003eFTIR spectrum of ZnO:MnO:VO composite samples.\u003c/p\u003e","description":"","filename":"5.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6304051/v1/1fc051cd9eda869abfcacb89.jpg"},{"id":79867856,"identity":"88cf0a5f-18e4-4950-bf41-1e19bcfaa10a","added_by":"auto","created_at":"2025-04-03 19:47:09","extension":"jpg","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":112134,"visible":true,"origin":"","legend":"\u003cp\u003eCV curves of ZnO:MnO:VOelectrode-based supercapacitor\u003c/p\u003e","description":"","filename":"6.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6304051/v1/3053621fef89d6650d0c88b2.jpg"},{"id":79867626,"identity":"1561a483-03d2-4f73-b8ec-510c10b3c2a6","added_by":"auto","created_at":"2025-04-03 19:39:09","extension":"jpg","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":103304,"visible":true,"origin":"","legend":"\u003cp\u003eGCD curves of ZnO:MnO:VOelectrode-based supercapacitor\u003c/p\u003e","description":"","filename":"7.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6304051/v1/669b6498a340872b576eca46.jpg"},{"id":79867618,"identity":"62d2b235-de66-4ef6-98f8-57bd045d3ae7","added_by":"auto","created_at":"2025-04-03 19:39:09","extension":"jpg","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":31823,"visible":true,"origin":"","legend":"\u003cp\u003eNyquist plots of Zn-Mn-VO with Equivalent circuit\u003c/p\u003e","description":"","filename":"8.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6304051/v1/f6928c456e70977e80e2ec27.jpg"},{"id":83555301,"identity":"7de3a9d5-57c4-496f-9699-f90ff411696a","added_by":"auto","created_at":"2025-05-28 11:32:04","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1489694,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6304051/v1/f912b46b-af6b-4345-841a-c7445b6a7e3a.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Synthesis and Electrochemical Performance of ZnO:MnO:VO Ternary Metal Oxide Nanocomposite for Supercapacitor Applications","fulltext":[{"header":"Introduction","content":"\u003cp\u003eAdvanced research on supercapacitor electrode materials has been intensified because industries worldwide need better and greener energy storage techniques. Supercapacitors demonstrate their importance as fundamental parts in renewable energy systems and portable electronics along with hybrid electric vehicles because they have excellent characteristics such as rapid charge-discharge rates and up to 10 kW/kg power density along with cycle stability exceeding 1,000,000 cycles[\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e]. Superconductors have a small energy density of 5 to 10 Wh/kg that restricts their broader usage compared to batteries[\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. The solution to this challenge demands new strategies that will enhance the specific capacitance and extend the potential window range of electrode materials.\u003c/p\u003e \u003cp\u003eSuperior energy storage functions of supercapacitors has been developed through the incorporation of transition metal oxides like MnO₂, ZnO and VOₓ. The pseudocapacitive applications of MnO₂ benefit from abundant studies because of its high theoretical specific capacitance value at 1370 F/g alongside economical prices [\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. The theoretical capacitance of ZnO stands high at ~\u0026thinsp;750 F/g while its environmental compatibility serves as an advantage for its use in energy storage devices[\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]. Among various advantages of vanadium oxides (VOₓ) lie the capability to shift between V⁵⁺ \u0026harr; V\u0026sup3;⁺ valence states which results in rapid charge transfer and high energy density up to ~\u0026thinsp;400 Wh/kg[\u003cspan additionalcitationids=\"CR6\" citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. These materials alone face implementation hurdles because of their inadequate electrical transmission and their poorly stable repeated charge-discharge cycles[\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e, \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e]. The development of composite materials through several integrated transition metal oxides creates synergistic characteristics to address the existing challenges[\u003cspan additionalcitationids=\"CR11 CR12 CR13 CR14\" citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. Research has shown that hydrothermal reaction techniques enable the synthesis of Mn-Cu-Ni composites which perform well in terms of specific capacitance alongside cycling stability verification[\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e]. Trimetallic fluorides which contain Ni-Co-Zn have demonstrated outstanding achievement with their high specific capacitance values and extended cyclic durability[\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e]. The research confirms that combined multi-component systems have the ability to improve charge storage alongside cyclic performance durability[\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe production and characterization of ZnO:MnO:VO (1:1:1 molar wt.) nanocomposite powders are described in detail based on hydrothermal processing then thermal treatment steps. The nanocomposite contains MnO as a main redox capacity contributor with ZnO serving as an environmentally friendly substance and VO providing multiple charge storage characteristics. Different techniques such as X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy and Fourier-transform infrared spectroscopy and transmission electron microscopy were used to characterize the synthesized materials. System performance measurements used cyclic voltammetry as well as galvanostatic charge-discharge tests and electrochemical impedance spectroscopy. Evaluation outcomes indicate that the ZnO:MnO:VO combination exists as a promising material for supercapacitor applications using advanced storage technologies for upcoming energy solutions.\u003c/p\u003e"},{"header":"Experimental Section","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003eSynthesis of material\u003c/h2\u003e \u003cp\u003eThe synthesis of ZnO:MnO:VO (1:1:1) nanocomposite powder started with preparing 50 mL of 0.1 M solutions by dissolving ammonium metavanadate (NH₄VO₃, 2.18 g) and manganese acetate tetrahydrate [(CH₃COO)₂Mn\u0026middot;4H₂O, 2.44 g] together with zinc acetate dihydrate [Zn(CH₃COO)₂\u0026middot;2H₂O, 1.16 g] in distilled water. The mixture of precursors received 5 mL of Polyethylene glycol (PEG) which later underwent 30 minutes of stirring with a magnet at room temperature to achieve mixture uniformity. The solution received a transfer into a 250 mL Teflon-lined stainless steel autoclave for hydrothermal treatment at 100\u0026deg;C over a period of 16 hours. The precipitate was separated through centrifugation at 5000 rpm for 5 minutes and this process was performed several times (4 to 5 repetitions) before washing with ethanol and distilled water until pH became neutral. The ZnO:MnO:VO nanocomposites were produced by subjecting the product to six hours of calcination at 300\u0026deg;C under air conditions.\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eMaterial characterization\u003c/h3\u003e\n\u003cp\u003eThe analysis of synthesized samples through X-ray diffractometry (Panalytical Xpert Pro) utilized CuKα radiation (k\u0026thinsp;=\u0026thinsp;1.54 \u0026Aring;) for a 2θ Bragg angle range from 10\u0026deg; to 80\u0026deg; to determine both crystallinity and phase composition. The Perkin Elmer instrument was used for FTIR spectroscopy to detect functional groups that exist in the material. EDS from Bruker analyzed the elemental content of the material while SEM from GEOL M-MUJ served to study the high magnification surface topography of the material. TEM analysis using Tachnai 200 Model generated images that showed clear grain boundaries while detecting thin dislocations occurring inside the grains. The EmStat4S electrochemical workstation operated GCD and CV and EIS tests on the materials. The EDLCs required CV evaluation through multiple scan rates between 0 and 0.8 V utilizing values of 3, 5, and 7 mV s\u0026thinsp;\u0026minus;\u0026thinsp;1. At different current densities between 2 and 5 A g\u0026thinsp;\u0026minus;\u0026thinsp;1 and within the potential range of 0\u0026ndash;0.8 V the GCD experiment occurred. EIS analysis spanned frequencies from 0.01 Hz to 100 kHz.\u003c/p\u003e\n\u003ch3\u003eFabrication of Electrodes\u003c/h3\u003e\n\u003cp\u003eTo make the working electrode, 80% of the Zn-Mn-V oxide nanocomposite was mixed with 10% polyvinylidene fluoride (PVDF) and 10% acetylene black (AB). This mixture was then turned into a paste using N-methyl-2-pyrrolidone (NMP) as the solvent.Then, the prepared paste was evenly spread over a 1 \u0026times; 1 cm\u0026sup2; area of the graphite sheet. The coated electrode was dried in the oven at 80\u0026deg;C for 12 hours to make sure everything sticks properly and the solvent evaporates.\u003c/p\u003e"},{"header":"Results and Discussion","content":"\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003eX-ray Diffraction (XRD)\u003c/h2\u003e \u003cp\u003eX-ray diffraction (XRD) was utilized to investigate the crystalline structure and phase composition of the synthesized ZnO:MnO:VO. XRD measurements were performed using a Panalytical with Cu Kα radiation (λ\u0026thinsp;=\u0026thinsp;1.54060 \u0026Aring;) over a 2θ range from 10\u0026deg; to 80\u0026deg;. The XRD pattern exhibited distinct peaks at 2θ values of 18.75, 24.23, 30.40, 36.28, 38.18, 40.41, 52.75, 53.68, 64.90, which were indexed to the (100), (110), (111), (200), (002), (211), (220), (311), (222) respectively. The MnO (FCC) major peaks are identified as (111), (200), (220), (311) and confirmed by JCPDS No. 75\u0026ndash;0626[\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e], ZnO (Wurtzite, Hexagonal) major peaks are found (100), (101), (102) confirmed by JCPDS No. 36-1451[\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e] and VO Orthorhombic at (110 ) JCPDS 41-1426[\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e]. To assess the lattice parameters, the diffraction angles for the prominent peaks were used to calculate the d-spacing values using Bragg\u0026rsquo;s law.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe crystallite size of the synthesized ZnO:MnO:VO nanocomposite was calculated using the Scherrer equation:\u003cdiv id=\"Equa\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equa\" name=\"EquationSource\"\u003e\n$$\\:D=\\frac{\\text{K}{\\lambda\\:}}{{\\beta\\:}\\text{c}\\text{o}\\text{s}{\\theta\\:}}$$\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003ewhere D is the crystallite size, K is the shape factor (0.9), λ is the X-ray wavelength (0.154 nm), β is the FWHM (full width at half maximum), and θ is the Bragg angle. The calculated crystallite sizes ranged from 1.50 nm to 3.71 nm, indicating the formation of fine crystalline grains. Specific values include 3.57 nm at 18.7572\u0026deg;, 1.50 nm at 24.2304\u0026deg;, and 3.71 nm at 36.2807\u0026deg;, with other peaks corresponding to crystallite sizes between these ranges[\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. The absence of additional peaks associated with impurity phases confirms the high phase purity of the material. The XRD results demonstrate the successful synthesis of the ZnO:MnO:VO nanocomposite with well-defined crystalline characteristics, providing valuable insights into its structural properties and potential electrochemical applications.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003eScanning Electron Microscopy (SEM)\u003c/h2\u003e \u003cp\u003eThe SEM analysis provides detailed insights into the surface morphology of the sample. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e, displays the SEM images of the ZnO:MnO:VO nanocomposite at different magnifications, revealing a well-defined nanorod morphology[\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e]. In Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e(a) at 30,000x magnification, the nanorods exhibit diameters ranging from 80\u0026ndash;120 nm and lengths of approximately 500\u0026ndash;700 nm, with smooth surfaces and sharp edges, indicating uniform crystal growth. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e(b) at 10,000x magnification shows the agglomeration of nanorods into hierarchical structures, which enhances the surface area and may improve electrochemical performance. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e(c) at 5,000x magnification further highlights the interconnected nanorods, suggesting homogeneous dispersion across the composite[\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e]. At 2,000x magnification in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e(d), a broader field of view confirms the uniform distribution of nanorods throughout the sample[\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e]. The absence of significant structural defects across all scales indicates the successful synthesis of a highly crystalline ZnO:MnO:VO nanocomposite, which is suitable for supercapacitor and energy storage applications.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eEnergy-Dispersive X-ray (EDX)\u003c/h3\u003e\n\u003cp\u003eThe EDX analysis of the ZnO:MnO:VO nanocomposite confirms the presence of oxygen (O), vanadium (V), manganese (Mn), and zinc (Zn), which are the primary constituents of the composite. The quantitative analysis reveals that vanadium is the most dominant element, accounting for 41.0 wt.%, followed by manganese (34.4 wt.%), oxygen (15.6 wt.%), and zinc (9.0 wt.%). The detected elemental ratios align closely with the expected composition, confirming the successful incorporation of these metal oxides during the hydrothermal synthesis and subsequent calcination[\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. The absence of any additional peaks in the EDX spectrum indicates high purity of the synthesized composite without any contamination or unwanted secondary phases. The elemental mapping images further illustrate the spatial distribution of each element across the sample surface. The oxygen (O) map (Figure a) reveals a homogeneous distribution, confirming the presence of metal oxides uniformly dispersed throughout the nanocomposite matrix[\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e]. The zinc (Zn) map (Figure b) shows a well-scattered, consistent distribution, supporting the successful incorporation of the ZnO phase[\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e, \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. The vanadium (V) map (Figure c) displays a uniform spread of vanadium, confirming its successful incorporation and even dispersion within the composite[\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e]. Similarly, the manganese (Mn) map (Figure d) indicates an even and widespread presence of manganese, which aligns with the significant contribution of the MnO phase identified by XRD[\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e]. The consistent and uniform distribution of all these elements suggests homogeneity within the nanocomposite, which is essential for achieving superior electrochemical performance[\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e\n\u003ch3\u003eTransition Electron Microscope (TEM)\u003c/h3\u003e\n\u003cp\u003eIn Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e (a) TEM imaging reveals the presence of well-defined nanorod with lengths 585 nm and diameter is 65 nm, confirming a rod-like morphology. The nanorod length and width were calculated by ImageJ software. The Selected Area Electron Diffraction (SAED) pattern from the Transmission Electron Microscope (TEM) confirms a crystalline structure with distinct diffraction spots and concentric rings, indicating a polycrystalline nature in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e(b)[\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e]. Image analysis identified eight prominent diffraction rings, with calculated d-spacing values of 0.118 nm, 0.081 nm, 0.063 nm, 0.057 nm, 0.050 nm, 0.044 nm, 0.040 nm, and 0.037 nm, derived using the provided scale of 5.00 1/nm[\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e]. The observed d-spacing values closely align with the face-centered cubic (FCC) structure, particularly the (111), (200), and (220) planes, which have characteristic d-spacings of 0.202 nm, 0.143 nm, and 0.117 nm, respectively. Additionally, the measured 0.118 nm corresponds to the (211) plane of the body-centered cubic (BCC) structure, which also includes 0.203 nm (110) and 0.144 nm (200). However, the data does not match the typical d-spacings of the hexagonal close-packed (HCP) structure, reinforcing the dominance of FCC and potential BCC phases. The crystallite size was calculated using the Debye-Scherrer equation from both the SAED and XRD patterns[\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e]. The TEM-SAED analysis yielded a crystallite size range of 2.10 nm to 4.05 nm, which slightly exceeds the XRD-based estimation of 1.50 nm to 3.71 nm, suggesting the presence of fine, highly crystalline grains. The SAED results align closely with X-ray Diffraction (XRD) findings, where reflections at 18.75\u0026deg;, 24.23\u0026deg;, 30.40\u0026deg;, and 36.28\u0026deg; correspond to the (111), (200), (220), and (311) planes of the MnO (FCC) phase, confirmed by JCPDS No. 75\u0026ndash;0626. The SAED-derived d-spacings support the identification of the FCC structure and match the key reflections observed in XRD. The clear and uniform diffraction rings indicate a high degree of crystallinity with minimal structural defects.[\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e, \u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e] Furthermore, comparison with crystallographic databases supports the presence of ZnO (Wurtzite, Hexagonal) and VO (Orthorhombic) phases, though their contributions are less pronounced in the SAED pattern. This comprehensive analysis confirms the successful synthesis of the ZnO:MnO:VO composite with high crystallinity and phase purity, as evidenced by the strong agreement between SAED and XRD results.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003eFTIR\u003c/h2\u003e \u003cp\u003eThe FTIR spectrum of the ZnO:MnO:VO nanocomposite provides insight into the functional groups and metal-oxygen bonding present in the material. The broad absorption band observed around 3350 cm⁻\u0026sup1; corresponds to the O-H stretching vibration of hydroxyl groups, indicating the presence of residual moisture or surface-adsorbed water [\u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e]. This is common in metal oxide nanomaterials due to their high surface area. The weak band near 1634 cm⁻\u0026sup1; can be attributed to the H-O-H bending vibration, further confirming adsorbed water molecules[\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e]. The V\u0026ndash;O stretching vibrations that give rise to a substantial peak reaching 816.42 cm⁻\u0026sup1; indicate the presence of vanadium oxides (VOₓ) and V\u0026ndash;O\u0026ndash;M linkages which include zinc or manganese metals (M)st[\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e40\u003c/span\u003e]. The qualitative analysis shows that the composite contains successfully incorporated vanadium units. A group of strong peaks located between 500\u0026ndash;600 cm⁻\u0026sup1; identifies the Zn\u0026ndash;O and Mn\u0026ndash;O stretching bonds indicating that zinc oxide (ZnO) and manganese oxide (MnO) phases have formed[\u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e41\u003c/span\u003e, \u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e]. Research findings from mixed metal oxides demonstrate an agreement with current results which confirms the presence of all desired phases[\u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]. The FTIR analysis reveals no major organic peaks because the organic residues successfully removed throughout the calcination step. The nanocomposite ZnO:MnO:VO succeeds in its formation as confirmed through characteristic peaks which indicate strong metal-oxygen bonding[\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e]. The successful synthesis of well-defined ZnO:MnO:VO nanocomposite was validated through FTIR analysis which supplemented the XRD and TEM-SAED results. The extensive characterizations reveal all the necessary features for this material to demonstrate promising energy storage performance because strong metal-oxygen bonds combined with structural stability enhance electrochemical performance.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec12\" class=\"Section2\"\u003e \u003ch2\u003eElectrochemical Performance:\u003c/h2\u003e \u003cp\u003eEvaluation of ZnO:MnO:VO nanocomposite electrode electrochemical performance levels required electrochemical test execution. The aqueous electrolytes allow voltage operation between 0.8V because electrolysis occurs beyond this limit. The electrochemical testing process of ZnO:MnO:VO electrode based supercapacitors involved 1M KOH aqueous electrolyte solutions tested through \u0026minus;\u0026thinsp;0.4V to 0.4V potential. Compositional ratio of synthesis material, binder and conducting material and electrolytes was 80:10:10 employed to create electrodes for the assembly of device. The binder PVDF provide mechanical qualities to carbon particles, but they also contribute the electrode material's electric and ionic resistance, limiting the device's power capabilities, due to that reason conducting materials are used to compensate ionic and electric resistance [\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e].\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec13\" class=\"Section2\"\u003e \u003ch2\u003eCyclic voltammetry (CV)\u003c/h2\u003e \u003cp\u003eA CV analysis was performed through various scan rates between 3 mVs⁻\u0026sup1; to 7 mVs⁻\u0026sup1; and a potential scope from \u0026minus;\u0026thinsp;0.4V to 0.4V. The capacitor typical curve appears in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e. A perfect CV curve profile with symmetrical shapes adjacent to zero current appears on the ZnO:MnO:VO cells when the scan rate remains low indicating quick and reversible charge and discharge processes without redox reactions. Raising the scan rate does not alter the symmetrical appearance of the CV indicating the charging process maintains consistency with the discharging process. The size of the CV area grows bigger as the scan rate increases since faster scan rates result in greater ion concentration. This affects the device's performance. The energy storage capacity grows larger because the ions accelerate their movement within electrolyte pores[\u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e46\u003c/span\u003e]. The specific capacitance measurements from cyclic voltammetry reached 232.11, 195.41, and 178.42 Fg⁻\u0026sup1; at the different scan rates between 3, 5, and 7 mVs⁻\u0026sup1;. The research data shows that specific capacitance diminishes when the scan rate grows higher. The electrode active sites are easier to reach by ions when scan rates remain low thus permitting better ion insertion. The measurement of higher capacitance occurs at scan rates that remain low.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec14\" class=\"Section2\"\u003e \u003ch2\u003eGalvanostatic charge-discharge (GCD)\u003c/h2\u003e \u003cp\u003eA near-symmetrical triangular shape represents the GCD curves of the supercapacitor constructed with ZnO:MnO:VO electrodes as per Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e. The capacitive behavior and operating efficiency of the supercapacitor appear excellent based on this result. The symmetric cells received specific capacitance calculation using a stated formula found in reference [\u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e47\u003c/span\u003e].\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ1\" name=\"EquationSource\"\u003e\n$$\\:{C}_{s}=2\\frac{I\\varDelta\\:T}{m\\varDelta\\:U}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e1\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eThe measurement combines m for mass of one electrode with I as current and has two time intervals Δt and potential range ΔU.\u003c/p\u003e \u003cp\u003eFigure \u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e shows the GCD curves at different current densities (2, 3, 4, and 5 A/g) at 0.8V. The calculated specific capacitances were 222.75 F/g, 213.37 F/g, 197 F/g, and 178.75 F/g for the corresponding current densities of 2, 3, 4, and 5 A/g.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec15\" class=\"Section2\"\u003e \u003ch2\u003eElectrochemical Impedance Spectroscopy (EIS)\u003c/h2\u003e \u003cp\u003eTo understand the mobility or limitation of ion transport in porous architecture of ZnO:MnO:VO, EIS was also performed. Figure\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e depicts the Nyquist fitted plots for fabricated of ZnO:MnO:VO electrode device with in a frequency range of 0.01 Hz to 100 KHz to determine the charge transfer process. The straight line in the Nyquist spectra indicates a low charge transfer resistance of electrode material's with excellent pseudocapacitive properties [\u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e46\u003c/span\u003e, \u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e47\u003c/span\u003e]. The measurement technique incorporates all resistive elements into the electrolyte resistance (Rs). Electrolyte resistance and charge transfer resistance show low levels in the intervals of low frequency according to the Nyquist plot data. Studies have shown that ZnO:MnO:VO develops electrolyte resistances (Rs) equal to 11.4Ω. Nanoparticles of ZnO:MnO:VO exhibit electrodes with low resistance which offer simple pathways for charge intercalation and de-intercalation between the electrode and electrolyte according to ESI results. Zsimpwin 3.20 software enabled the fitting process which established R1(C1R2)(Q1R3)(C2R4) as the equivalent Randles circuit for the cells. Few of the various cell resistances have been named R1, R2, R3, R4 respectively. The equivalent Randles circuit for the cell uses R2 as grain resistance while R1 represents Ohmic contact resistance and R4 and R3 stand for sample\u0026ndash;electrode interface and grain boundary resistance. The sub-circuit Q1R3 contains a constant phase element Q1 while C1 along with C2 represent parallel capacitances within C1R2 and C2R4 components respectively. Grain resistance (R2) becomes lower as the frequency increases yet the interface resistance (R4) and grain boundary resistance (R2) show a rising pattern according to frequency changes.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"Conclusion","content":"\u003cp\u003eThe ZnO:MnO:VO nanocomposite is successfully synthesized through hydrothermal processing followed by calcination which contains MnO (FCC), ZnO (Wurtzite, Hexagonal) and VO (Orthorhombic). The XRD results showed highly crystalline structures with crystallite dimensions between 1.50 nm to 3.71 nm and the FTIR patterns matched with metal-oxygen functional bonds. SEM showed that nanocomposite materials presented rod-shaped features extending from 1 \u0026micro;m to 10 \u0026micro;m while elemental distribution across the structure was verified through EDX examination. The structural stability together with purity and dimensional control of the composite indicates its suitability for use in supercapacitors and additional energy storage systems. The electrochemical performance of the ZnO:MnO:VO nanocomposite was evaluated using cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS) in 1M KOH aqueous electrolyte. The specific capacitance found by CV and GCD analysis was 232.11 Fg⁻\u0026sup1; and 222.75 Fg⁻\u0026sup1; respectively. Hence, the structural and morphological properties of ZnO:MnO:VO nanocomposite are suitable for high capacitive supercapacitor.\u003c/p\u003e"},{"header":"Declarations","content":" \u003cp\u003e \u003cstrong\u003eCompeting Interests\u003c/strong\u003e \u003cp\u003eThe authors declare no competing interests.\u003c/p\u003e \u003c/p\u003e\u003ch2\u003eFunding\u003c/h2\u003e \u003cp\u003eThere is no financial support was received for the research, authorship or publication of this manuscript.\u003c/p\u003e\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eCRediT authorship contribution statementRekha Kumari : Writing \u0026ndash; original draft, Methodology, Investigation, Formal analysis. Vivek Kumar Shukla: Writing \u0026ndash; original draft, review\u0026amp; SupervisionYogesh Kumar: Writing \u0026ndash; review \u0026amp; editing\u003c/p\u003e\u003ch2\u003eAcknowledgement\u003c/h2\u003e \u003cp\u003eOne of the authors Rekha Kumari acknowledge the University Grant Commission (UGC), India for providing her financial support through JRF fellowship in this duration and Dr. Anurag Tyagi for scientific discussions.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eDissanayake K, Kularatna-Abeywardana D (2024) A review of supercapacitors: Materials, technology, challenges, and renewable energy applications. 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Materials Science for Energy Technologies 3:289\u0026ndash;298. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.mset.2019.11.004\u003c/span\u003e\u003cspan address=\"10.1016/j.mset.2019.11.004\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Supercapacitors, ZnO:MnO:VO, Ternary Metal Oxide, Hydrothermal synthesis, XRD, SEM, EDX, FTIR, TEM, CV, GCD and EIS","lastPublishedDoi":"10.21203/rs.3.rs-6304051/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6304051/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThis investigation describes both the synthesis process and detailed inspection of ZnO:MnO:VO nanocomposites which were made through hydrothermal processing and subsequent heating treatment. X-ray diffraction results showed that the prepared nanocomposite structure primarily contained the FCC phase of MnO and small amounts of Wurtzite ZnO and Orthorhombic VO phases. The nanocomposite contains tiny crystalline grains rabged from 1.50 to 3.71 nm, as determined through the Debye-Scherrer formula. The characteristic FTIR vibrational modes from metal-oxygen (M\u0026ndash;O) bonds validated the composite formation in the analysis. The Scanning Electron Microscope showed rod-shaped components with lengths from 1 \u0026micro;m to 10 \u0026micro;m and Energy Dispersive X-ray Spectroscopy demonstrated that all four atomic elements of Zn, Mn and V and O existed evenly throughout the composite structure. The structural analysis showed strong crystalline content and complete phase purity because no additional impurities were present. The electrochemical assessment of the ZnO:MnO:VO nanocomposite took place through CV and GCD and EIS testing in 1M KOH aqueous electrolyte. The specific capacitance by CV and GCD analysis were found 232.11 Fg⁻\u0026sup1; and 222.75 Fg⁻\u0026sup1; respectively. The structural and morphological properties of ZnO:MnO:VO nanocomposite are suitable for supercapacitor applications and finds high capacitive devices.\u003c/p\u003e","manuscriptTitle":"Synthesis and Electrochemical Performance of ZnO:MnO:VO Ternary Metal Oxide Nanocomposite for Supercapacitor Applications","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-04-03 19:39:04","doi":"10.21203/rs.3.rs-6304051/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"311a2035-770e-42cb-af2e-cda777004b02","owner":[],"postedDate":"April 3rd, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2025-05-28T11:23:40+00:00","versionOfRecord":[],"versionCreatedAt":"2025-04-03 19:39:04","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-6304051","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6304051","identity":"rs-6304051","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}