Cyclic Voltammograms Research Articles

Boron-Salphen Conjugate based Molecular Probe Exhibiting Fluorescence On-Off-On Response in Detection of Cu2+ and ATP through Displacement Approach.

Synthesis and photophysical properties of a fluorescent probe HBD is described. Probe upon interaction with metal ions, anions and nucleoside pyrophosphates (NPPs) showed fluorescence quenching with Cu2+ due to chelation enhanced quenching effect (CHEQ). Moreover, interaction of ensemble HBD.Cu2+ with anions and NPPs showed fluorescence "turn-On" response with ATP selectively. "On-Off-On" responses observed with Cu2+ and ATP is attributed to an interplay between ESIPT and TICT processes. Cyclic voltammogram of probe exhibited quasi-reversible redox behaviour with three oxidation and two reduction potentials and the change in band gaps of probe suggested the interaction with Cu2+ and ATP. The 2 : 1 and 1 : 1 binding stoichiometry for an interaction between probe and Cu2+ (LOD, 62 nM) and ensemble, HBD.Cu2+ with ATP (LOD, 0.4 μM) respectively are realised by Job's plot and HRMS data. Cell imaging studies carried out to detect Cu2+ and ATP in HeLa cells. Also, the output emission observed with Cu2+ and ATP is utilized to construct an implication (IMP) logic gate. Test paper strips showed naked-eye visible color responses to detect Cu2+ and ATP. In real water samples probe successfully detected copper (0.03 μM) between 5-6.5 ppb level (ICP-MS method).

Design of a Rotating Disk Electrode setup operating under high pressure and temperature: Application to CO2 reduction on gold

We describe the design and development of a rotating disk electrode (RDE) cell capable of operating at pressures up to 200 bar and temperatures up to 200 °C. This setup enables electrochemical surface characterization through techniques such as voltammetry and impedance spectroscopy, under different mass transport regimes. Furthermore, evaluation of catalytic performance, including CO2 reduction, is possible as the system works in a semi-continuous mode interfaced with online gas sample measurements. As a proof of concept of the high-pressure cell designed, we examined the temperature-dependent changes in the cyclic voltammograms (CVs) of polycrystalline gold up to 150 °C and 50 bar. Additionally, online catalytic performance of CO2 reduction to CO on a rotating polycrystalline gold disk electrode was investigated under different pressure and temperature. Our results indicate a positive impact of temperature on the faradaic efficiency (FE) towards CO up to 50 °C, beyond which a rapid drop in performance was observed at atmospheric pressure. Conversely, increasing pressure positively affected CO2 solubility in the electrolyte, resulting in enhanced FE towards CO, reaching approximately 90 % at 6 bar compared to 40 % at atmospheric pressure. Notably, further increases in pressure did not significantly alter the FE, but led to higher current densities. Moreover, at pressures exceeding 6 bar, we observed a plateau in efficiency at temperatures higher than 50 °C. This observation suggests that increasing pressure can sustain CO2 electrolysis, validating the hypothesis that increasing CO2 solubility would suppress catalytic decay at higher temperatures. This study opens up promising avenues for future investigations in electrocatalysis, ranging from fundamental explorations of surface modifications induced by variations in temperature and pressure to the development of high-performance catalysts.

A comparative study of graphene-based electrodes for electrochemical detection of visceral leishmaniasis in symptomatic and asymptomatic patients

BackgroundVisceral Leishmaniasis is a neglected tropical disease with a high rate of infection and mortality in affected areas. Around 50,000 to 90,000 new cases of visceral leishmaniasis (VL) are estimated every year. Individuals asymptomatic for the disease should also be considered in epidemiological surveillance of the disease, as they can help spread the parasite. Thus, the development of low-cost diagnosis methods that allow the identification of infected and asymptomatic individuals is required, especially in developing countries where this disease is endemic. ResultsIn this work, we developed an immunosensor for recognizing anti-Leishmania antibodies in asymptomatic individuals and avoiding cross-reaction with Chagas disease (CD). For that, we used carbon-based screen-printed electrodes, modified with graphene oxide and gold. Reproducibility was assessed by calculating the relative standard deviation (RSD < 5 %) from cyclic voltammograms of [Fe(CN)6]3-/4− using three different electrodes, screen-printed carbon electrodes (DPR-110) and graphene modified screen-printed electrodes (DPR-110 GPH) were purchased from DropSens (Oviedo, Asturias, Spain). SignificanceAs an electrochemical methodology, we use cyclic voltammetry. After the tests were carried out, we considered that carbon electrodes adsorbed with reduced graphene oxide and modified with gold nanoparticles were the best platforms for detecting anti-Leishmania antibodies. In the study carried out, the limit of quantification (LOQ) for anti-Leishmania antibodies was established at 16.75 mg/mL, while the limit of detection (LOD) was 5.58 mg/mL. These limits indicate the minimum antibody concentration values that can be quantified and detected accurately and reliably in the analyzed sera.

Reduced graphene oxide/zinc oxide composite as an electrochemical sensor for acetylcholine detection

Acetylcholine (ACh) plays a pivotal role as a neurotransmitter, influencing nerve cell communication and overall nervous system health. Imbalances in ACh levels are linked to neurodegenerative diseases, such as Alzheimer's and Parkinson's. This study focused on developing electrochemical sensors for ACh detection, utilizing graphene oxide (GO) and a composite of reduced graphene oxide and zinc oxide (rGO/ZnO). The synthesis involved modified Hummers' and hydrothermal methods, unveiling the formation of rGO through deoxygenation and the integration of nano-sized ZnO particles onto rGO, as demonstrated by XPS and TEM. EIS analysis also revealed the enhancement of electron transfer efficiency in rGO/ZnO. Cyclic voltammograms of the electrode, comprising the rGO/ZnO composite in ACh solutions, demonstrated prominent oxidation and reduction reactions. Notably, the composite exhibited promise for ACh detection due to its sensitivity, low detection threshold, reusability, and selectivity against interfering compounds, specifically glutamate and gamma-aminobutyric acid. The unique properties of rGO, such as high specific surface area and electron mobility, coupled with ZnO's stability and catalytic efficiency, contributed to the composite's potential in electrochemical sensor applications. This research, emphasizing the synthesis, fabrication, and characterization of the rGO/ZnO composite, established itself as a reliable platform for detecting the acetylcholine neurotransmitter.

Rice powder template for hausmannite Mn3O4 nanoparticles and its application to aqueous zinc ion battery.

In this study, a simple calcination route was adopted to prepare hausmannite Mn3O4 nanoparticles using rice powder as soft bio-template. Prepared Mn3O4 was characterized by Fourier Transform Infra-Red Spectroscopy (FTIR), Field Emission Scanning Electron Microscopy (FESEM), Energy Dispersive X-ray microanalysis (EDX), Powder X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM), Brunauer-Emmett-Teller (BET) and Solid state UV-Vis spectroscopic techniques. Mn-O stretching in tetrahedral site was confirmed by FTIR and Raman spectra. % of Mn and O content supported Mn3O4 formation. The crystallinity and grain size was found to be 68.76% and 16.43 nm, respectively; tetragonal crystal system was also cleared by XRD. TEM clarified the planes of crystal formed which supported the XRD results and BET demonstrated mesoporous nature of prepared Mn3O4 having low pore volume. Low optical band gap of 3.24 eV of prepared Mn3O4 nanoparticles indicated semiconductor property and was used as cathode material to fabricate CR-2032 coin cell of Aqueous Rechargeable Zinc Ion Battery (ARZIB). A reversible cyclic voltammogram (CV) showed good zinc ion storage performance. Low cell resistance was confirmed by Electrochemical Impedance Spectroscopy (EIS). The coin cell delivered high specific discharge capacity of 240.75 mAhg-1 at 0.1 Ag-1 current density. The coulombic efficiency was found to be 99.98%. It also delivered excellent capacity retention 94.45% and 64.81% after 300 and 1000 charge-discharge cycles, respectively. This work offers a facile and cost effective approach for preparing cathode material of ARZIBs.

Evaluation of Scan Rate Influence on Cyclic Voltammograms of Copper Electrodes Coated with PS-CS-GA/ZnO Nanocomposite

Evaluation of Scan Rate Influence on Cyclic Voltammograms of Copper Electrodes Coated with PS-CS-GA/ZnO Nanocomposite

Screening of Pd-Co-Ni catalyst arrays by scanning electrochemical microscopy and characterization of the potential catalyst for formic acid oxidation

BackgroundAppropriate anodic catalyst is one of the key points in improving the performance of direct formic acid fuel cells (DFAFCs). This study utilizes the concept of a combination method to design and screen anodic catalysts for formic acid oxidation. MethodsThe tip generation-substrate collection (TG-SC) mode of scanning electrochemical microscopy (SECM) was employed to screen the Pd-Co-Ni ternary catalyst array for catalyzing formic acid oxidation. The potential catalyst was further characterized by scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). Significant findingsThe composition ratios of the prepared Pd-Co-Ni ternary catalyst array matched the concentration ratios set by the precursor solution. SECM screening revealed that the optimal ratio for formic acid oxidation was the Pd2Co6Ni2 catalyst. The cyclic voltammograms and CO stripping voltammograms indicate that the Pd2Co6Ni2 electrode exhibits lower onset potentials for the oxidation of formic acid and its intermediates than the pure Pd electrode. Electrochemical impedance spectroscopy (EIS) confirms that the Pd2Co6Ni2 electrode possesses lower interfacial resistance than the Pd electrode, with its pseudo-inductive behavior at high potential aligning with the outcomes observed in cyclic voltammograms and CO stripping voltammograms.

Tailored PEO synthesis and in-situ ATR-FTIR study of PtSnO2/Nb coral-like structures for application in ethanol electrooxidation

Coupling the electrooxidation of organic compounds (EOO) with hydrogen evolution can be a sustainable way for green hydrogen production, and therefore it’s of great interest to the development of suitable electrocatalysts for efficient EOO. In this study, we present the successful solvothermal synthesis of a Pt-based electrocatalyst for an ethanol oxidation reaction (EOR), using a coral-like structure as substrate which was prepared by plasma electrolytic oxidation (PEO) on a metallic niobium. Chemical analysis revealed the predominance of SnO2 in the PEO structure, while Pt doping demonstrated selectivity on the surface of the electrocatalyst. Cyclic voltammograms indicate a high electrochemically active surface area (122.45 m² gPt−1), with an onset potential of 0.27 V vs. SHE. In-situ spectroelectrochemical analysis confirm the efficient ethanol electrooxidation with remarkable selectivity in C-C bond cleavage. The prepared electrocatalyst stands out as a promising contribution to advances in green hydrogen production by coupling EOR with hydrogen evolution.

M(TEIM) complexes with M as Co and Fe: Analogues of classic M(TIM)

The syntheses and characterization of Fe and Co complexes supported by a new tetra-imine macrocycle, TEIM (2,3,9,10-tetraethyl-1,4,8,11-tetraazacyclotetradeca-1,3,8,10-tetraene), are reported. Templating with Co(OAc)2·4H2O yielded trans-[Co(TEIM)Cl2][PF6] (1a), which was converted to trans-[Co(TEIM)X2][PF6] (X = N3 (2a) and NO2 (3a)) through reactions with NaX (X = N3 or NO2). Templating with Fe generated trans-[Fe(TEIM)(NCCH3)2][PF6]2, which was oxidized to trans-[Fe(TEIM)Cl2][PF6] (1b). The reaction of 1b with NaN3 formed [Fe(TEIM)(N3)2][PF6] (2b) while the reaction with [Fe(TEIM)(NCCH3)2][PF6]2 and NaNO2 yielded trans-[Fe(TEIM)(NO2)2] (3b). Single crystal X-ray diffraction studies revealed a pseudo-octahedral geometry around the Co / Fe centers with the ethyl groups oriented above or below the plane of the TEIM ring. The absorption spectra of 1b displays weak charge transfer bands near the UV to visible region, while 2b and 3b displayed intense charge transfer bands within the visible region. Cyclic voltammograms of 1a revealed four 1 e− reductions while those of 2a and 3a display only three cathodically shifted reductions. Analogous studies of 1b and 2b revealed two 1 e- reductions while 3b displays only an oxidation event. EPR studies of ferric complexes 1b and 2b indicated a low spin d5 electronic figuration with S = ½ ground state.

Electrochemical study of cerium and iron doped MoO3 nanoparticles showing potential for supercapacitor application

This study presents the synthesis and comprehensive characterization of undoped MoO3 and its cerium (Ce) and iron (Fe) doped counterparts via hydrothermal route, with a 5 % doping concentration. Structural analysis by X-ray diffraction confirmed the formation of MoO3 with successful doping. UV–vis spectroscopy demonstrated tunable optical properties, with band gap energies of 2.3 eV, 2.0 eV, and 2.8 eV for undoped, Ce-doped and Fe-doped MoO3 respectively. Morphological investigation using scanning electron microscopy revealed distinct nanostructures, including nanorods, agglomerated nanoparticles, and pebble-like structures, influenced by doping. Electrochemical characterization through cyclic voltammetry and potentio electrochemical impedance spectroscopy showcased superior charge storage capacity in Fe-doped MoO3, attributed to the largest area under the curve in cyclic voltammograms. Fe-doped MoO3 exhibited lowest resistance as compared to undoped and Ce doped MoO3, suggesting enhanced conductivity. The presence of a Warburg element in all samples indicated diffusion-limited electrochemical processes. The variation of log (scan rate) with log (current) revealed distinct charge transfer mechanisms, with near-unity slopes for doped samples and a slope near 0.5 for undoped MoO3. These findings provide insights into the tunable properties of doped MoO3, offering potential applications in various electrochemical devices.

Fabrication of nickel aluminate based electrochemical sensor for dopamine detection

Nickel aluminate nanoparticles (NiAl2O4 NPs) spinel structure is synthesized via a simple solution combustion method using aqueous nickel nitrate, aluminum nitrate and citric acid. The crystal structure and microstructure of the prepared NiAl2O4 NPs are confirmed by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectrum, scanning and transmission electron microscopy (SEM/TEM). The characterized NiAl2O4 NPs are applied on a glassy carbon electrode (GCE) to design electrochemical sensor for the detection of dopamine (DA) using cyclic voltammograms (CV) and differential pulse anodic stripping voltammograms. The proposed electrochemical sensor exhibits excellent sensing activity with a low detection limit of 1.78 μM and applicable for a wide linear concentration range of 10 μM–140 μM. Further, the proposed electrode exhibits well resolved differential pulse voltammogram for the dopamine in presence of interfering uric acid and ascorbic acid.

Optimization of the structural, optical, and photovoltaic characteristics of a novel ruthenium(III) complex as a photosensitizer for solar cells

A novel ruthenium(III) complex, [Ru(DAP)2(H2O)2]Cl3 (where DAP = 5,6-Diamino-1,3-dimethylpyrimidine-2,4(1H,3H)-dione), was synthesized for potential application as a photosensitizer dye in solar cell. The ruthenium complex was made and precipitated as violet crystals by reaction of K2[RuCl5H2O] with the ligand DAP, in an aqueous ethanol (1:1; v/v)). Elemental analysis, magnetic, thermal, X-ray diffraction, electron scanning microscope and spectroscopic techniques were used for physico-chemical characterizations. Additionally, the electrochemical properties were studied by cyclic voltammetry and voltammogram showed different peaks with different oxidation potentials confirming an extraordinary electrochemical property for the complex. The fabrication of nanostructured films of ruthenium(III) complex was achieved through the thermal evaporation technique, and from which optical and electrical characterizations were studied and interpreted. A solar cell hybridizing organic and inorganic materials, incorporating a ruthenium(III) complex and silicon, was fabricated. The current-voltage characteristic of this cell was measured, and from which the photovoltaic parameters were estimated. The solar cell exhibits a filling factor of 0.40 and an efficiency of 3.58 %.

Structural, bandgap tailoring, photoluminescence and electrochemical characteristics of Sm3+-doped ZnS quantum dots prepared in Ar-atmosphere

Sm3+-doped ZnS quantum dots were prepared by a cost-effective, simple co-precipitation technique under an argon atmosphere. The prepared Sm3+-doped QDs exhibited a cubic structure with an average particle size of ∼ 2 nm, as confirmed through X-ray diffraction and high-resolution transmission electron microscopic investigations. The crystallite was reduced and strain produced due to the larger ionic radius of Sm3+ ions. The Sm (at. 2 %)-doped ZnS exhibited a blue shift, and the optical transmittance was enhanced. A highly intense red emission was obtained in photoluminescence investigations, and this is due to the transfer of photons from 4G5/2 → 6H11/2 for f-f transitions of the Sm3+ in the 4f5 configuration. The obtained photoluminescence emissions lead to red phosphor applications. The cyclic voltammogram analysis showed that adding Sm to ZnS QDs made their specific capacitance value higher and it found potential applications in supercapacitors.

Synthesis, Spectroscopic, and DFT Studies of Vanadium (III) Hydroxamate Complex with Potential Biological Applications

A new vanadium (III) hydroxamate complex of composition V(4- NO2C6H4CH=CHCONHO)3 has been synthesized by reaction of VCl3 with potassium salt of 4-nitrocinnamohydroxamate (4-NO2C6H4CH=CHCONHO) in 1:3 molar ratio in dry methanol solvent. The newly synthesized complex is characterized by elemental analysis, molar conductivity, magnetic moment measurements and IR, UV-Vis spectral studies and mass spectrometry. DFT calculations were carried out by using Orca 4.2.1 program and the negative values of the energies of EHOMO and ELUMO for the V(III) complex confirm its stability. A distorted-octahedral geometry around vanadium center has been suggested for complex based upon physicochemical, spectroscopic and DFT studies, involving bonding through hydroxylamine and carbonyl oxygens (O O coordination). The cyclic voltammogram of the complex shows single anodic and cathodic peak. The TGA/DTA curve indicates the single step decomposion of complex. The biological potential of the ligand and complex have been tested by in vitro antimicrobial studies and cytotoxicity assay. Antimicrobial activity of complex has been found increased as compare to precursor and ligand. The results of cytotoxicity reveal the complex less toxic as compared to standard drug simvastatin.

Concerted Two-Proton-Coupled Electron Transfer from Piceatannol to Electrogenerated Superoxide in N,N-Dimethylformamide.

The reactivity of 4-[(E)-2-(3,5-dihydroxyphenyl)ethenyl]benzene-1,2-diol (piceatannol) toward electrochemically generated superoxide radical anion (O2 •-) was investigated using electrochemistry and in situ controlled-potential electrolytic electron spin resonance (ESR) measurements in N,N-dimethylformamide with density functional theory (DFT) calculations. The quasireversible cyclic voltammogram of dioxygen/O2 •-, modified in the presence of piceatannol, indicated that the electrogenerated O2 •- was scavenged by piceatannol via proton-coupled electron transfer. Differences in the reactivities of piceatannol and 5-[(E)-2-(4-hydroxyphenyl)ethen-1-yl]benzene-1,3-diol (trans-resveratrol) toward O2 •-, originating from the presence of the benzene-1,2-diol (catechol) moiety, were observed in the voltammograms and ESR measurements. The electrochemical and computational results show that the reaction mechanism is a concerted two-proton-coupled electron transfer (2PCET) via the catechol moiety of piceatannol. The stilbene moiety of piceatannol kinetically promotes 2PCET via its catechol moiety. These findings indicate that piceatannol is a better O2 •- scavenger than catechol and trans-resveratrol.

Introducing Novel Redox-Active Bis(phenolate) N-Heterocyclic Carbene Proligands: Investigation of Their Coordination to Fe(II)/Fe(III) and Their Catalytic Activity in Transfer Hydrogenation of Carbonyl Compounds.

A simple and efficient procedure for synthesizing novel pincer-type tridentate N-heterocyclic carbene bisphenolate ligands is reported. The synthesis of pincer proligands with N,N'-disubstituted imidazoline core, 5 and 6, was carried out via triethylorthoformate-promoted cyclization of either N,N'-bis(2-hydroxy-3,5-di-tert-butylphenyl)cyclohexanediamine, 3, or N,N'-bis(2-hydroxyphenyl)cyclohexanediamine, 4, in the presence of concentrated hydrochloric acid. Cyclic voltammograms of the ligands revealed ligand-centered redox activity, indicating the noninnocent nature of the ligands. The voltammograms of the ligands exhibit two successive one-electron oxidations and two consecutive one-electron reductions. In contrast to previous reports, the redox-active ligands in this study exhibit one-electron oxidation and reduction processes. All products were thoroughly characterized by using 1H and 13C NMR spectroscopy. The base-promoted deprotonation of the proligands and subsequent reaction with iron(II) and iron(III) chlorides yielded compounds 7 and 8. These compounds are binuclear and tetranuclear iron(III) complexes that do not contain carbene functional groups. Complexes 7 and 8 were characterized by using elemental analysis and single-crystal X-ray crystallography. At low catalyst loadings, both 7 and 8 exhibited high catalytic activity in the transfer hydrogenation of selected aldehydes and ketones.

An affordable and green voltammetric approach for the determination of sotalol in biological, environmental, and pharmaceutical samples

AbstractThis work outlines the development of a voltammetric method for a sensitive, rapid, and environmentally friendly determination of the antihypertensive sotalol (SOT) in several sample types employing the anodically pretreated boron‐doped diamond electrode. Cyclic voltammograms of SOT presented a well‐defined irreversible oxidation peak at 1.21 V (Ag/AgCl (3.0 mol L−1 KCl)) in Britton–Robinson buffer solution (pH 3.0). Figures of merits recommended by the validation guidelines were evaluated for the validation of the present method. Employing differential pulse voltammetry linearity of SOT was obtained in the concentration range of 0.39–4.22 μmol L−1 in 0.1 mol L−1 H2SO4 solution, with a limit of detection of 0.031 μmol L−1. The selectivity of the method was assessed against interferers and show relative standard deviation (RSD) values lower than 6 %. Recovery tests yielded percentages ranging from 93 % to 96 % in urine sample and from 100 % to 107 % in tap water sample. The proposed method was successfully applied in pharmaceutical, environmental, and biological samples offering a suitable green analytical chemistry profile.

Structure and electrochemical properties of D-glucose-derived hard carbon as a negative electrode in potassium-ion batteries

Hard carbons (HC) have been synthesized from D-glucose and pectin via a hydrothermal technique and pyrolized at 1200°C, 1400°C and 1600°C. Their structural evolution depending on the pyrolysis temperature was investigated with X-ray powder diffraction, Raman spectroscopy with additional characterization with scanning and transmission electron microscopy and gas adsorption/desorption measurements. More ordered and uniform structures were obtained at higher pyrolysis temperature. Correlations of the HC structure with the electrochemical properties as a negative electrode (anode) in potassium half-cells and interaction mechanism of K+ ions with HC were analyzed and discussed. The prevalence of pseudocapacitive contribution for K-ion interaction with HC was deduced from cyclic voltammograms. The hydrothermally pre-treated HC anodes annealed at higher temperature demonstrate less pseudocapacitive and more pronounced diffusion-controlled behavior causing a capacity decrease with increasing pyrolysis temperature from 277 mAh/g (1200°C) to 243 mAh/g (1400°C) and to 153 mAh/g (1600°C).

Effect of temperature on the chemical activation of carbon nanospheres and their efficiency in supercapacitors

We report the synthesis of carbon spheres (CSs) by pyrolysis of soybean oil and their chemical activation employing acid baths at different temperatures. This allows to study the effect of these experimental parameters on the efficiency of these materials for their use as supercapacitor electrodes. The CSs were characterized by SEM, Raman, XRD, FT-IR, BET, and TEM to reveal the relationship between the electrochemical properties and the structure. Using nitric acid as the activating agent causes the formation of micropores and a high density of oxygenated functional groups in the CSs. In contrast, the mixture of sulfuric and nitric acids destroys the CSs, producing coalescence. The capacitance of the CSs was ~103 F g−1 at 5 mV s−1, and the contribution of electrical double-layer capacitance and pseudocapacitance was determined using cyclic voltammograms. Moreover, it is observed that after 1000 galvanostatic charge-discharge cycles at 2 A g−1, the CSs with the larger electrochemical capacitance increase their capacitive performance up to 38 %, maintaining the electrical double-layer capacitance contribution constant. Therefore, we show that controlling the density of oxygenated functional groups anchored through an increase in temperature during acid treatment and generating high surface areas are key parameters to obtain high capacitance.

Design of a new nanocomposite based on Keggin-type [ZnW12O40]6− anionic cluster anchored on NiZn2O4 ceramics as a promising material towards the electrocatalytic hydrogen storage

Extensive research efforts have been dedicated to developing electrode materials with high capacity to address the increasing complexities arising from the energy crisis. Herein, a new nanocomposite was synthesized via the sol–gel method by immobilizing K6ZnW12O40 within the surface of NiZn2O4. ZnW12O40@NiZn2O4 was characterized by FT-IR, UV–Vis, XRD, SEM, EDX, BET, and TGA-DTG methods. The electrochemical characteristics of the materials were examined using cyclic voltammogram (CV) and charge–discharge chronopotentiometry (CHP) techniques. Multiple factors affecting the hydrogen storage capacity, including current density (j), surface area of the copper foam, and the consequences of repeated cycles of hydrogen adsorption–desorption were evaluated. The initial cycle led to an impressive hydrogen discharge capability of 340 mAh/g, which subsequently increased to 900 mAh/g after 20 cycles with a current density of 2 mA in 6.0 M KOH medium. The surface area and the electrocatalytic characteristics of the nanoparticles contribute to facilitate the formation of electrons and provide good diffusion channels for the movement of electrolyte ions throughout the charge–discharge procedure.