Ternary Electrocatalysts Research Articles

One-Pot Fast Electrochemical Synthesis of Ternary Ni-Cu-Fe Particles for Improved Urea Oxidation

The climate crisis has become the most serious concern of human beings and environments worldwide in the 21st century. Global concerns about cancer epidemiology mainly originate from anthropogenic activities, particularly fossil-based operations. A key solution to this problem is the use of fuel cells—devices—capable of the direct conversion of fuel chemical energies like urea into electricity. To make their commercialization reasonable, one of the problems that needs to be solved is the development of anodic materials. The majority of investigations on urea oxidation are based on nickel, but its inadequate activity limits the efficiency of these devices. In this work, we propose and synthesize a Ni-Cu-Fe ternary electrocatalyst for urea oxidation through a fast and facile electrodeposition method. The properties of the synthesized material are examined by Scanning Electron Microscopy (SEM) conjugated with Energy Dispersive X-ray Spectroscopy (EDS), Transmission Electron Microscopy (TEM), and X-ray Diffraction (XRD). Its electrochemical properties were also examined in a 1 M KOH solution with and without 0.15 M urea. We found that the prepared powder is active in the electro-oxidation of urea, with 1.65 Vvs RHE required for a current density of 10 mA cm−2 and a stable potential of 2.38 Vvs RHE required for 3 h of polarization at 10 mA cm−2.

Novel mixed heterovalent (Mo/Co)Ox-zerovalent Cu system as bi-functional electrocatalyst for overall water splitting

A novel hybrid ternary metallic electrocatalyst of amorphous Mo/Co oxides and crystallized Cu metal was deposited over Ni foam using a one-pot, simple, and scalable solvothermal technique. The chemical structure of the prepared ternary electrocatalyst was systematically characterized and confirmed via XRD, FTIR, EDS, and XPS analysis techniques. FESEM images of (Mo/Co)Ox–Cu@NF display the formation of 3D hierarchical structure with a particle size range of 3–5 µm. The developed (Mo/Co)Ox–Cu@NF ternary electrocatalyst exhibits the maximum activity with 188 mV and 410 mV overpotentials at 50 mA cm−2 for hydrogen evolution reaction (HER) and oxygen evolution reaction (OER), respectively. Electrochemical impedance spectroscopy (EIS) results for the (Mo/Co)Ox–Cu@NF sample demonstrate the minimum charge transfer resistance (Rct) and maximum constant phase element (CPE) values. A two-electrode cell based on the ternary electrocatalyst just needs a voltage of about 1.86 V at 50 mA cm−2 for overall water splitting (OWS). The electrocatalyst shows satisfactory durability during the OWS for 24 h at 10 mA cm−2 with an increase of only 33 mV in the cell potential.

Self-Standing Metal Foam Catalysts for Cathodic Electro-Organic Synthesis.

Although electro-organic synthesis is currently receiving renewed interest because of its potential to enable sustainability in chemical processes to value-added products, challenges in process development persist: For reductive transformations performed in protic media, an inherent issue is the limited choice of metallic cathode materials that can effectively suppress the parasitic hydrogen evolution reaction (HER) while maintaining a high activity toward the targeted electro-organic reaction. Current development trends are aimed at avoiding the previously used HER-suppressing elements (Cd, Hg, and Pb) because of their toxicity. Here, this work reports the rational design of highly porous foam-type binary and ternary electrocatalysts with reduced Pb content. Optimized cathodes are tested in electro-organic reductions using an oxime to nitrile transformation as a model reaction relevant for the synthesis of fine chemicals. Their electrocatalytic performance is compared with that of the model CuSn7Pb15 bronze alloy that has recently been endorsed as the best cathode replacement for bare Pb electrodes. All developed metal foam catalysts outperform both bare Pb and the CuSn7Pb15 benchmark in terms of chemical yield and energetic efficiency. Moreover, post-electrolysis analysis of the crude electrolyte mixture and the cathode's surfaces through inductively coupled plasma mass spectrometry (ICP-MS) and scanning electron microscopy (SEM), respectively, reveal the foam catalysts' elevated resistance to cathodic corrosion.

Ni2P/Co2P as a highly efficient catalyst for enhancing the electrochemical performance of P-NiMoO4 for oxygen evolution reaction

A growing trend in electrocatalysis is to explore interfacial interactions and surface intermediate adsorption in highly efficient bimetallic phosphide catalysts for developing efficient oxygen evolution reactions (OER). In this work, Ni2P and Co2P nanoparticles (NPs) were distributed on P-modified NiMoO4 nanorods prepared by the hydrothermal procedure, which exhibited high catalytic activity and outstanding durability for the OER. By regulating the high interfacial contact between Ni2P, Co2P, and P-NiMoO4, the Ni2P and Co2P NPs reduced the electron density, thus optimizing the OER. Compared to the NiMoO4 NRs, the P-NiMoO4@Ni2P/Co2P electrocatalyst showed remarkable activity towards the OER owing to the strong electron interaction and synergistic effect among the three components. Consequently, the P-NiMoO4@Ni2P/Co2P electrode yielded significant OER activity, with an overpotential of 260 mV, a Tafel slope of 41 mV/dec, and 92.9% Faradaic efficiency. Furthermore, the P-NiMoO4@Ni2P/Co2P electrocatalyst demonstrated excellent stability (up to 50 h) for the OER, which was higher than those of the NiMoO4-based catalysts reported in the literature. Several factors contribute to the excellent OER activity, including electron transfer between Ni2P, Co2P, and P-NiMoO4, and the abundant active sites generated from their interfacial interactions. Therefore, this study presents a novel approach for developing highly efficient ternary electrocatalysts for the long-term electrocatalytic evolution of oxygen.

Bottom-up self-assembly strategy to construct ternary MoxC/Ni3Fe@GL as efficient water splitting electrocatalyst

Efficient and robust bifunctional non-precious metal electrocatalysts, used for oxygen evolution reaction (OER) and hydrogen evolution reaction (HER), are crucial to develop water splitting commercial applications. Herein, a bottom-up self-assembly strategy is proposed to construct ternary electrocatalysts of nitrogen-doped graphene-like carbon layers encapsulated MoxC (x = 1, 2) and Ni3Fe alloy nanoparticles (MoxC/Ni3Fe@GL) for efficient water electrolysis. The optimized sample (0.27MoxC/Ni1.5Fe@GL, 0.27 represent the mass of ammonium molybdate in the precursor) requires overpotentials (η10) of 88 and 150, 265 mV in 0.5 M H2SO4 for HER and 1.0 M KOH for HER and OER, respectively. Furthermore, as a bifunctional electrocatalyst in a two-electrode cell, 0.27MoxC/Ni1.5Fe@GL requires only 1.523 V at 10 mA cm−2, which surpasses the noble metal RuO2(+)||Pt/C(−) in 1.0 M KOH electrolyte, and shows excellent stability by working at 20 mA cm−2 long as 150 h. The superior electrocatalytic performance can mainly originate from MoxC and Ni3Fe alloys synergistically effected results. The partial doping of Ni or Fe atoms into Mo2C optimizes the electronic structure, making the intrinsic activity enhanced. On the other hand, the incorporation of MoxC heterophases effectively inhibits the Ni3Fe nanoparticles agglomeration, benefitting to expose more active sites. Moreover, the protection of encapsulated thin N-doped graphene-like carbon layers for the nanoparticles against corrosion, guarantees the long-time durability. This work provides a potential general bottom-up self-assembly approach to construct high-performance electrocatalysts with multiphase heterostructures with enriched abundant active sites and enhanced intrinsic activity for energy coversion fields.

Resolving Atomic-Scale Structure and Chemical Coordination in High-Entropy Alloy Electrocatalysts for Structure-Function Relationship Elucidation.

The recent breakthrough in confining five or more atomic species in nanocatalysts, referred to as high-entropy alloy nanocatalysts (HEAs), has revealed the possibilities of multielemental interactions that can surpass the limitations of binary and ternary electrocatalysts. The wide range of potential surface configurations in HEAs, however, presents a significant challenge in resolving active structural motifs, preventing the establishment of structure-function relationships for rational catalyst design and optimization. We present a methodology for creating sub-5 nm HEAs using an aqueous-based peptide-directed route. Using a combination of pair distribution function and X-ray absorption spectroscopy, HEA structure models are constructed from reverse Monte Carlo modeling of experimental data sets and showcase a clear peptide-induced influence on atomic-structure and chemical miscibility. Coordination analysis of our structure models facilitated the construction of structure-function correlations applied to electrochemical methanol oxidation reactions, revealing the complex interplay between multiple metals that leads to improved catalytic properties. Our results showcase a viable strategy for elucidating structure-function relationships in HEAs, prospectively providing a pathway for future materials design.

Postdecorated Polyoxometalate Metal–Organic Framework-Constructed Ternary Electrocatalysts for Hydrogen Evolution

Postdecorated Polyoxometalate Metal–Organic Framework-Constructed Ternary Electrocatalysts for Hydrogen Evolution

Machine learning filters out efficient electrocatalysts in the massive ternary alloy space for fuel cells

Despite their potential promise, multicomponent materials have not been actively considered as catalyst materials to date, mainly due to the massive compositional space. Here, targeting ternary electrocatalysts for fuel cells, we present a machine learning (ML)-driven catalyst screening protocol with the criteria of structural stability, catalytic performance, and cost-effectiveness. This process filters out only 10 and 37 candidates out of over three thousand test materials in the alloy core@shell (X3Y@Z) for each cathode and anode of fuel cells. These candidates are potentially synthesizable, lower-cost and higher-performance than conventional Pt. A thin film of Cu3Au@Pt, one of the final candidates for oxygen reduction reactions, was experimentally fabricated, which indeed outperformed a Pt film as confirmed by the approximately 2-fold increase in kinetic current density with the 2.7-fold reduction in the Pt usage. This demonstration supports that our ML-driven design strategy would be useful for exploring general multicomponent systems and catalysis problems.

Hybrid ternary NiCoCu layered double hydroxide electrocatalyst for alkaline hydrogen and oxygen evolution reaction

This study focuses on the electrochemical properties of layered double hydroxide (LDH), which is a specific structure of NiCoCu LDH, and the active species therein, rather than the oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) of ternary NiCoCu LDH materials. Six types of catalysts were synthesized using the reflux condenser method and coated onto a nickel foam support electrode. Compared to bare, binary, and ternary electrocatalysts, the NiCoCu LDH electrocatalyst exhibited higher stability. The double layer capacitance (Cdl) of the NiCoCu LDH (12.3 mF cm−2) is greater than that of the bare and binary electrocatalysts, indicating that the NiCoCu LDH electrocatalyst has a larger electrochemical active surface area. In addition, the NiCoCu LDH electrocatalyst has a lower overpotential of 87 mV and 224 mV for the HER and OER, respectively, indicating its excellent activity with the bare and binary electrocatalysts. Finally, it is demonstrated that the structural characteristics of the NiCoCu LDH contribute to its excellent stability in long-term HER and OER tests.

Nature-Inspired Design of Nano-Architecture-Aligned Ni5P4-Ni2P/NiS Arrays for Enhanced Electrocatalytic Activity of Hydrogen Evolution Reaction (HER)

The projection of developing sustainable and cost-efficient electrocatalysts for hydrogen production is booming. However, the full potential of electrocatalysts fabricated from earth-abundant metals has yet to be exploited to replace Pt-group metals due to inadequate efficiency and insufficient design strategies to meet the ever-increasing demands for renewable energies. To improve the electrocatalytic performance, the primary challenge is to optimize the structure and electronic properties by enhancing the intrinsic catalytic activity and expanding the active catalytic surface area. Herein, we report synthesizing a 3D nanoarchitecture of aligned Ni5P4-Ni2P/NiS (plate/nanosheets) using a phospho-sulfidation process. The durability and unique design of prickly pear cactus in desert environments by adsorbing moisture through its extensive surface and ability to bear fruits at the edges of leaves inspire this study to adopt a similar 3D architecture and utilize it to design an efficient heterostructure catalyst for HER activity. The catalyst comprises two compartments of the vertically aligned Ni5P4-Ni2P plates and the NiS nanosheets, resembling the role of leaves and fruits in the prickly pear cactus. The Ni5P4-Ni2P plates deliver charges to the interface areas, and the NiS nanosheets significantly influence Had and transfer electrons for the HER activity. Indeed, the synergistic presence of heterointerfaces and the epitaxial NiS nanosheets can substantially improve the catalytic activity compared to nickel phosphide catalysts. Notably, the onset overpotential of the best-modified ternary catalysts exhibits (35 mV) half the potential required for nickel phosphide catalysts. This promising catalyst demonstrates 70 and 115 mV overpotentials to attain current densities of 10 and 100 mA cm-2, respectively. The obtained Tafel slope is 50 mV dec-1, and the measured double-layer capacitance from cyclic voltammetry (CV) for the best ternary electrocatalyst is 13.12 mF cm-2, 3 times more than the nickel phosphide electrocatalyst. Further, electrochemical impedance spectroscopy (EIS) at the cathodic potentials reveals that the lowest charge transfer resistance is linked to the best ternary electrocatalyst, ranging from 430 to 1.75 Ω cm-2. This improvement can be attributed to the acceleration of the electron exchangeability at the interfaces. Our findings demonstrate that the epitaxial NiS nanosheets expand the active catalytic surface area and simultaneously elevate the intrinsic catalytic activity by introducing heterointerfaces, which leads to accommodating more Had at the interfaces.

Tuning the electrocatalytic performances of Ni-MOF with combined tungsten compounds (WO3-x/WS2-x) decorated rGO by interface coupling for efficient water oxidation

The novel design of noble metal-free electrocatalyst with new structure/combination and cost-effectiveness are vital sources for the featuring hydrogen energy sector (mainly hydrogen and oxygen evolution reaction (OER)) in the viewpoint of commercialization of water electrolyzers. Herein, we constructed a new kind of ternary rG-W-N electrocatalyst (reduced graphene oxide - a new formation of heterostructured tungsten compound W-O-S (WO3-x/WS2-x) - Ni-MOF) for enhancing the OER activity. Interestingly, the seeded W-O-S grew from inside of rGO layer with a spherical formation in binary composition. The excellent electrocatalyst for OER was identified by systematically investigating from the binary and ternary electrocatalysts using different concentrations. The homogeneous rG-W-N nanocomposite exhibits remarkable performance for water oxidation, with an ultra-low over potential value of 170 mV at 10 mA cm−2 towards OER performance. In addition, it shows an efficient stability performance after 5000 cycles. The rG-W-N electrocatalyst boosts the sluggish intermediate pathway for OER, which is the primary reason for attaining the lowest over potential. The electronic and synergetic effects in rG-W-N leads to interfacial interaction/connectivity between the ternary materials and large active sites enhance the efficient charge transfer reaction.

Ru decorated Pt2CoNi/C nanoparticles as a proficient electrocatalyst for oxygen reduction reaction

Exploring minimal usage and highly proficient cathode electrocatalyst for oxygen reduction is greatly lessening the expenditure incurred in low-temperature fuel cells. Herein, we report a simple solvothermal process for the synthesis of Ru-Pt 2 CoNi/C-2 as a doped ternary electro catalyst towards efficient oxygen reduction reaction (ORR). In present study, Ru-Pt 2 CoNi/C-2 catalyst exhibits a specific activity and mass activity of 1.6 mA/cm 2 Pt and 0.31 A/mg Pt , which is 8 and 2.2 times higher, when compared to commercial Pt/C catalyst correspondingly. Interestingly, the long-time durability test (up to 20k cycles) reveals the significant ORR stability of Ru-Pt 2 CoNi/C-2 catalyst with 75% retention in its specific activity (1.2 mA/cm 2 Pt ). Moreover, a 30% enhancement in the electrochemically active surface area (ECSA) was recorded after 20k cycles, due to the complete exposure of all underlying active sites during the potential cycling. • Study of Ruthenium (Ru) doped Pt ternary alloys to form Ru-Pt 2 CoNi/C-2 catalyst. • The oxophilic nature of Ru kinetically favours Oxygen Reduction Reaction. • I m and I s of Ru-Pt 2 CoNi/C-2 is 2.2 times and 8 times higher respectively than that of commercial Pt/C. • Ru-Pt 2 CoNi/C shows minimal loss (ΔE 1/2 = 5 mV) in activity after 20000 potential cycles.

Electrosynthesis of ternary nonprecious Ni, Cu, Fe oxide nanostructure as efficient electrocatalyst for ethanol electro-oxidation: Design strategy and electrochemical performance

Materials composed of various constituents with distinct physical or chemical features are named composites. Merging components in the composite structure leads to new properties creation or the intrinsic properties magnification of the components, or synergetic effects. Here, the ternary nanocomposite of copper, nickel, and iron oxides was electrodeposited on the glassy carbon electrode (GCE) surface to facilitate the ethanol electro-oxidation reaction (EOR) and overcome the electrode fouling problem while prolonging its efficiency. The GCEs were modified by three different procedures and activated by CV cycling in an alkaline solution, and their electro-catalytic activity was tested toward EOR. The ternary electrocatalysts prepared by two-steps electrodeposition of their components (Ni,Fe2O3/Cu and Cu/Ni,Fe2O3) demonstrated higher peak current and more negative peak potential (Epa = 476 mV, Ipa = 492 μA, and Epa = 510 mV, Ipa = 644 μA, respectively) than the binary electrocatalyst of Ni,Fe2O3 toward EOR. The best electro-catalytic efficiency was acquired for the simultaneous electrodeposition of nano Cu, Ni, and Fe2O3 on the GCE surface (Cu,Ni,Fe2O3, Epa = 530 mV, Ipa = 3179 μA). The physicochemical and electro-catalytic characterizations of the fabricated electrocatalysts were evaluated by various techniques. The fast and facile engineered design of the GCE modification with the ternary Cu,Ni,Fe2O3 components led to a high current density of about 101 mA/cm2 with increased tolerance against poisoning intermediates resulting in longtime stability for EOR in alkaline media. The synergistic effect between nano Ni, Cu, and Fe oxides provided promising properties for the EOR pursuing the construction of a powerful device with commercialization potential.

Enhanced electrocatalytic activity by NiCu-LDH/CoS as dual co-catalysts on g-C3N4 nanosheets in NiCu-LDH@CoS/g-C3N4 nanostructure for oxygen evolution reactions

The development of highly efficient electrocatalysts is crucial for realizing efficient oxygen evolution reactions (OERs). Herein, a novel strongly coupled ternary electrocatalyst of NiCu-layered double hydroxide (NiCu-LDH) on cobalt sulfide (CoS) and the material graphitic carbon nitride (g-C3N4) was synthesized. In OER tests, NiCu-LDH@CoS/g-C3N4 electrocatalyst exhibited excellent performance using 1 M KOH alkaline electrolyte. In the present study, the electrode potential was only 290 mV for a current density of 10 mA/cm2 and a Tafel slope of 75 mV/dec. The improved electrocatalytic activity was ascribed to the strong interaction and electronic coupling with efficient charge transfer at the CoS/g-C3N4 heterojunction interface and the enhanced electronic effects of NiCu-LDH at the NiCu-LDH@CoS/g-C3N4 interface. The optimized NiCu-LDH@CoS/g-C3N4 nanostructure was stable, with a 99.7% remarkable efficiency for the OER. This work presents a novel approach to maximize the efficiency through the synergetic effect of CoS and NiCu-LDH as dual co-catalysts for sustainable energy applications.

Efficient Ternary Cefecop Bifunctional Electrocatalyst for Overall Water Splitting

Efficient Ternary Cefecop Bifunctional Electrocatalyst for Overall Water Splitting

Bifunctional o-CoSe2/c-CoSe2/MoSe2 heterostructures for enhanced electrocatalytic and photoelectrochemical hydrogen evolution reaction

The bottleneck of alkaline hydrogen evolution reaction lies in the kinetically sluggish brought from multistep reaction processes involving water adsorption and dissociation, as well as hydrogen adsorption. In this work, we successfully synthesized o-CoSe2/c-CoSe2 heterostructures anchored on MoSe2 nanosheets to powerfully promote reaction processes. As an electrocatalyst, it exhibits a low overpotential of 112 mV at 10 mA/cm2 and a Tafel slope of 96.9 mV/dec for an alkaline hydrogen evolution reaction. Moreover, the as-prepared catalyst can behave as both cathode and anode for overall water splitting, which only requires 1.61 V cell voltage at 10 mA/cm2. Significantly, the cell voltage can be further reduced to 1.53 V at 10 mA/cm2 for water electrolysis under the simulated solar irradiation owing to such a semiconductor-based heterostructure that facilitates the separation of photogenerated charges. Here, the improving overall performance of this ternary electrocatalyst is attributed to the multifunctionality and synergistic interaction of different components in this heterogeneous material. The work provides a novel strategy to design active catalysts simultaneously using electric energy and solar energy for effective water splitting.

Pd-Pt nanoparticles combined with ceria nanorods for application in oxygen reduction reactions in alkaline direct ethanol fuel cell cathodes

Fuel cells are important energy conversion devices. However, challenges in this regard are still noted, such as low electrocatalyst efficiencies in the oxygen reduction reaction (ORR), which occurs slowly in electrocatalyst cathodes. In this sense, this study aimed to synthetize hybrid binary and ternary electrocatalysts formed by palladium and platinum alloy nanoparticles and ceria nanorods (CeO2 NR) supported on carbon black Vulcan XC-72 (PdxPty/Vn and (Pd3Pt1)x(CeO2 NR)y(Vn)z) for the study of the oxygen reduction reaction (ORR) and application as alkaline direct ethanol fuel cells (ADEFCs) cathodes. The binary and ternary hybrid electrocatalysts were characterized using different physicochemical and electrochemical techniques. The ternary hybrid electrocatalyst, (Pd3Pt1)15(CeO2 NR)10(Vn)75, reached higher open circuit voltage (OCV), maximum current and power densities, of 1.13 V, 219 mA cm-2 and 61 mW cm-2, respectively, compared to the commercial Pt/C Alfa Aesar (AA) and other evaluated electrocatalysts. The ternary hybrid electrocatalyst, (Pd3Pt1)15(CeO2 NR)10(Vn)75, is interesting for application as an ADEFC cathode targeting the ORR, due to an almost 3-fold maximum power density and almost twice the maximum current density compared to a commercial electrocatalyst with the same noble metal loading, explained by increased defects and oxygenated species in this electrocatalyst as revealed by Fourier Transform Infrared Spectroscopy (FT-IR) and Raman analyses.

Electrocatalysts based on low amounts of palladium combined with tin nanoparticles and cerium dioxide nanorods for application as ADEFC anodes

This study demonstrates the structural properties and evaluates the electrocatalytic activity of an ethanol oxidation reaction using ternary materials composed by Pd and Sn nanoparticles combined with CeO2 nanorods (NR) anchored on Vulcan carbon black to be used as an anode in alkaline direct ethanol fuel cells (ADEFCs). The highest open circuit voltage (1010 mV), maximum power (30 mW cm−2) and current densities (113 mA cm−2) were achieved using (Pd1Sn3)10(CeO2 NR)20(Vn)70, while the commercial anode values were 968 mV, 23 mW cm−2 and 123 mA cm−2. Although similar performance for both anodes was observed, the ternary hybrid electrocatalyst contains an 8-fold lower Pd content than the commercial material. This outcome may be justified by the higher defect density presented by the carbon support observed by Raman spectroscopy and the metal oxidation state modifications detected by X-ray photoelectron spectroscopy, as well as the electrochemically active surface area presented by the ternary electrocatalyst. The combination of higher vacancies, defects and oxygenated species in the carbon support and the synergistic effect between the oxyphilic Sn and CeO2 NR species and the Pd nanoparticles results in an electrochemical performance that makes these ternary electrocatalysts promising anode materials for ADEFC applications.

High-performing nanocatalyst screened via machine learning and confirmed experimentally

In this issue of Chem Catalysis , Han and co-workers combine first-principles calculations with a machine-learning technique to search ternary electrocatalyst for oxygen reduction reaction. The predicted promising PtFeCu nanoparticles were validated by experimental tests, showing both higher activity and more durable stability than commercial Pt/C. In this issue of Chem Catalysis , Han and co-workers combine first-principles calculations with a machine-learning technique to search ternary electrocatalyst for oxygen reduction reaction. The predicted promising PtFeCu nanoparticles were validated by experimental tests, showing both higher activity and more durable stability than did commercial Pt/C.

Fabrication and characterization of enhanced hydrazine electrochemical sensor based on gold nanoparticles decorated on the vanadium oxide, ruthenium oxide nanomaterials, and carbon nanotubes composites.

This work describes the synthesis of mixed oxide film of vanadium and ruthenium by pulsed deposition technique on multiwall carbon nanotubes and the decoration of gold nanoparticles on the mixed film. A ternary electrocatalyst has been developed for the electrochemical oxidation of hydrazine by combining two metal oxide mixtures with Au nanoparticles. Surface morphology and chemical composition of the electrode have been examined with SEM, EDX, HRTEM, EIS, and XRD. The peak current of hydrazine increased 9 times at the AuNPs/(VOx-RuOx)/CNT/GCE compared to the bare GCE, and the peak potential shifted to negative 848 mV. Linear sweep voltammetry (LSV) and amperometric techniques revealed that the AuNPs/(VOx-RuOx)/CNT/GCE displays linear concentration range 2.5–10000 µM (LSV) and the concentration range 0.03–100 µM (amperometry). The limit of detection (LOD) is 0.5 μM and 0.1 μM at (S/N = 3) for LSV and amperometric technique, respectively. The results obtained show a good RSD% of 2.1%–3.2% and reasonable recovery of 97%–108% of hydrazine detection.