Precise control over nanostructure evolution is critical for optimizing the electrochemical performance of pseudocapacitive materials. In this work, Nb₂O₅ nanostructures were synthesized via a time-engineered hydrothermal route by systematically varying the reaction duration (6, 12, and 18 h) to elucidate its influence on structural development, charge storage kinetics, and supercapacitor performance. Structural and surface analyses confirm the formation of phase-pure monoclinic Nb₂O₅ with a stable Nb⁵⁺ oxidation state. Morphological investigations reveal that a 12 h reaction time produces hierarchically organized Nb₂O₅ architectures composed of nanograin-assembled spherical aggregates with interconnected porosity, providing optimized ion diffusion pathways and enhanced electroactive surface exposure. Electrochemical evaluation demonstrates that the NbO-12 electrode delivers superior pseudocapacitive behavior dominated by diffusion-controlled Nb⁵⁺/Nb⁴⁺ redox reactions, exhibiting high areal capacitance (5.504 F cm⁻² at 8 mA cm⁻²), fast ion diffusion kinetics, low internal resistance, and excellent cycling stability with 85.73% capacitance retention over 12,000 cycles. Furthermore, an asymmetric pouch-type supercapacitor assembled using NbO-12 as the positive electrode and activated carbon as the negative electrode operates stably over a wide voltage window of 1.5 V, delivering an energy density of 0.101 mWh cm⁻² with outstanding durability. This study establishes hydrothermal reaction-time engineering as an effective strategy for tailoring Nb₂O₅ nanostructures and provides valuable insights for the rational design of high-performance pseudocapacitive electrodes for advanced energy storage systems.

The rational design of electrode materials with tailored composition and architecture is crucial for advancing high-capability electrochemical energy storage systems. This study reports that gadolinium-modified NiFe₂O₄ nanosheet electrodes were effectively synthesized on nickel foam via a hydrothermal approach followed by thermal treatment. A series of compositions (NiFe, NiFe–Gd1, NiFe–Gd2, and NiFe–Gd3) were prepared to systematically examine the effect of Gd incorporation on structural features and electrochemical properties. X-ray diffraction (XRD) analysis confirmed the formation of the cubic spinel NiFe₂O₄ phase without detectable secondary phases, indicating that the crystal structure remains intact after Gd introduction. X-ray photoelectron spectroscopy (XPS) further verified the presence of Ni²⁺, Fe³⁺, and Gd³⁺ species within the lattice environment. Morphological analysis using field-emission scanning electron microscopy (FESEM) revealed a nanosheet-based architecture, where the optimized NiFe–Gd2 electrode exhibited a porous and interconnected nanosheet framework with abundant exposed edges. This structural configuration improves electrolyte penetration and facilitates efficient ion transport during charge storage processes. Electrochemical measurements demonstrated that the NiFe–Gd2 electrode delivers an areal capacitance of 5235 mF cm⁻² at 10 mA cm⁻², along with improved reaction kinetics and low internal resistance. An asymmetric supercapacitor assembled using NiFe–Gd2 as the positive electrode and activated carbon as the negative electrode operated stably within a 0–1.5 V potential window, achieving an energy density of 0.136 mWh cm⁻² and a power density of 3.14 mW cm⁻², while retaining 86.55% of its initial capacitance after 7000 cycles. These results highlight the potential of rare-earth engineering as a viable strategy for designing advanced spinel ferrite electrodes and pave the way for the development of high-performance, durable, and scalable supercapacitor systems for practical energy storage applications.

This study presents a dual surfactant-assisted hydrothermal approach for the synthesis of Co₃V₂O₈ (CoVO) nanostructures and their surfactant-modified derivatives, PVP-assisted Co₃V₂O₈ (P-CoVO) and PVP–SDS co-assisted Co₃V₂O₈ (P/S-CoVO), which were directly grown on nickel foam. The use of PVP and SDS enabled controlled nucleation and growth, yielding a hierarchical nanoflower-like morphology in P/S-CoVO with increased porosity, a higher surface area, and uniform structural features. Comprehensive physicochemical characterization confirmed that surfactant incorporation effectively modulated particle size, dispersion, and active-site availability. Electrochemical measurements demonstrated that P/S-CoVO exhibited superior performance, with the largest CV area, low equivalent series resistance (0.52 Ω), and a maximum areal capacitance of 13.71 F cm⁻² at 8 mA cm⁻², attributable to rapid redox kinetics and efficient ion transport. The electrode also showed excellent cycling stability, retaining approximately 83.7% of its initial capacitance after 12,000 charge–discharge cycles, indicating robust structural integrity and interfacial stability. Additionally, an asymmetric supercapacitor device (P/S-CoVO//AC) delivered a high energy density of 0.082 mWh cm⁻², a power density of 1.25 mW cm⁻², and stable operation within a 1.5 V potential window. These results demonstrate that cooperative surfactant engineering provides an effective and scalable strategy to enhance the morphology, electrochemical kinetics, and durability of Co₃V₂O₈-based electrodes for next-generation high-performance supercapacitors.