Electrocatalytic Surface Research Articles

A global design principle for polysulfide electrocatalysis in lithium–sulfur batteries—A computational perspective

AbstractWidespread commercialization of high‐energy‐density lithium–sulfur (Li–S) batteries is difficult due to the lithium polysulfide, Li2Sn (n = 4, 6, 8), shuttle effect. Efficient adsorption/conversion of Li2Sn species on an electrocatalytic surface can suppress the shuttle effect. Modeling of the adsorption of Li2Sn species using density functional theory (DFT) calculations has contributed significantly toward an understanding of their anchoring mechanism at a surface. Different surfaces show a unique range of binding energies for faster Li2Sn adsorption/reaction kinetics. To predict the optimum binding energy zone, a systematic DFT study is performed on transition‐metal sulfide (TMS) surfaces including TiS2, VS2, NbS2, MoS2, WS2, and SnS2. The investigation revealed that the geometric properties at the anchoring site possibly regulate the adsorption energy of Li2Sn species. A geometry parameter, Gscore, is defined as a function of bond length and number of lithium‐atom interactions between the Li2Sn species and the binding surface. The design principle is extended to sulfur‐deficient (TMSs‐x) and edge‐exposed (TMS(100)) surfaces. The Gscore predicts the most effective binding energy zone distinctive to these materials—TMS (1.7–2.1 eV/Gscore ≥ 2.0), TMSs‐x (2.0–2.8 eV/Gscore ≥ 2.1), and TMS(100) (2.5–3.2 eV/Gscore ≥ 1.09).

Ferroelectric Modulation of Surface Electronic States in BaTiO3 for Enhanced Hydrogen Evolution Activity.

Ferroelectric nanomaterials offer the promise of switchable electronic properties at the surface, with implications for photo- and electrocatalysis. Studies to date on the effect of ferroelectric surfaces in electrocatalysis have been primarily limited to nanoparticle systems where complex interfaces arise. Here, we use MBE-grown epitaxial BaTiO3 thin films with atomically sharp interfaces as model surfaces to demonstrate the effect of ferroelectric polarization on the electronic structure, intermediate binding energy, and electrochemical activity toward the hydrogen evolution reaction (HER). Surface spectroscopy and ab initio DFT+U calculations of the well-defined (001) surfaces indicate that an upward polarized surface reduces the work function relative to downward polarization and leads to a smaller HER barrier, in agreement with the higher activity observed experimentally. Employing ferroelectric polarization to create multiple adsorbate interactions over a single electrocatalytic surface, as demonstrated in this work, may offer new opportunities for nanoscale catalysis design beyond traditional descriptors.

Black phosphorous dots phosphatized bio-based carbon nanofibers/bimetallic organic framework as catalysts for oxygen evolution reaction

As a multi-step and more complex half-cell reaction than the hydrogen reverse evolution reaction (HER), the oxygen evolution reaction (OER) always requires a higher overpotential than HER. In order to minimize the associated energy loss as an overpotential, these electrochemical half-reactions of water splitting should be catalyzed by suitable materials. Due to the abundant exposed surface area and extensive active edge sites, black phosphorous quantum dots (BP QDs) have shown great potential in OER. Here, BP QDs was introduced to incorporate with bio-based carbon nanofibers (CNF) and Co–Ni bimetallic organic framework (CoNiMOF), preparing a novel catalyst for oxygen evolution reaction (OER) by a facile one-pot reaction (Scheme 1). The unique structures and greater BET surface areas of CoNiMOF-BP QDs/CNF could possibly supply a larger electrocatalytic surface, expose further active sites. The obtained CoNiMOF-BP QDs/CNF possesses excellent electrocatalytic activity in alkaline electrolyte (1 M KOH) with a low overpotential of 281 mV at 10 mA cm−2 and a low Tafel slope of 111.9 mV dec−1. The CoNiMOF-BP QDs/CNF can remain stable for 25,000 s under alkaline electrolyte, showing excellent stability. The increase of electrocatalyst activity is mainly attributed to the synergistic effect of excellent conductivity and enriched active sites arising from BP QDs. This work not only provides an effective strategy for the development of bimetallic MOFs derived electrocatalysts, but also puts forward a new insight for the application of BP QDs in water splitting.

Three-dimensional hierarchical flowers-like cobalt-nickel sulfide constructed on graphitic carbon nitride: Bifunctional non-noble electrocatalyst for overall water splitting

Tailoring various micro-nano structured materials by employing different techniques to enhance their porosity and conductivity has captivated significant consideration, making their remarkable electrochemical properties accessible within the area of energy storage devices. Herein we report the impact of graphitic carbon nitride concentration (0.03 ∼ 0.1 g) on nickel-cobalt sulfide morphologies and performance in hydrogen production. Employing the facile hydrothermal method, a cubic crystalline nickel-cobalt sulfide was stabilized on defective layered graphitic carbon nitride nanosheets for overall water splitting. A performance peak was observed in a sample with a graphitic carbon nitride concentration of 50 mg, which not only prevented the agglomeration but also provided a porous structure for enhanced gas diffusivity and charge transfer rates owing to the synergistic Carbon and Nitrogen bonding with Cobalt and Nickel Sulfide. Optimized concentration of graphitic carbon nitride also increased the electrocatalytic active surface area threefold when compared with nickel-cobalt sulfide. The fabricated well-aligned flower-like pattern CoNi2S4/graphitic carbon nitride (50 mg) delivered a low overpotential of 310 mV and 160 mV for oxygen evolution reactions and hydrogen evolution reactions to reach a current density of 30 mA/cm2 and 10 mA/cm2 in alkaline media. The electrolyzer displayed an electrolysis potential of 1.58 V to reach 10 mA/cm2 current density with the long-term durability of 24 h. This strategy depicts a novel approach for utilizing this renowned nickel-cobalt sulfide with graphitic carbon nitride catalyst for the application of alkaline electrocatalytic water splitting.

Revealing failure modes and effect of catalyst layer properties for PEM fuel cell cold start using an agglomerate model

We propose a dynamic model for cold start of proton exchange membrane fuel cell in account for transport, phase-change and electrochemical reactions within catalyst agglomerates. The competition between loss of in-agglomerate reactant concentrations and active electro-catalytic surface is shown to cause different failure modes dependent on start-up current densities. Critical ice fractions of failure were identified for different cathode catalyst layer (CL) thickness and ionomer to carbon ratios (I/C) at 0.4 A cm−2. In contrast to thicker CLs that uplift the critical ice fraction, larger I/Cs decrease the CL porosity and agglomerate pore size, thus significantly reducing the critical ice fraction. Moreover, by utilizing the electro-osmotic drag effect, slightly thickening anode CLs provides effective internal heat source during cold start at high current densities with minimal impact on the nominal cell performance.

Novel syntheses of modified black TiO2/C3N4 and their efficient behavior toward water splitting under neutral conditions

Black titania (BT) incorporated carbon nitride (C3N4) nanoparticles; synthesized with imidazole and titania P-25 for the first time, without washing steps, was then loaded with 3 wt% of Ag2O, Ag2S, and CuO nanoarchitecture through a deposition hydrothermal route. The obtained electrocatalyst CuO/BT offers abundant active sites composed of TiO2−x@TiO2 interfaced with C3N4; that has been emphasized via various physicochemical techniques, besides the Cu+/Cu++ moieties, thus providing an exceptional electrocatalytic performance (configured using CV, LSV, EIS, and ECSA) under both neutral (KCl, pH = 7) and dark conditions. The overall water electrolysis to produce 10 mA cm−2 requires a potential of 1.7 V. This electrode exhibits a superior efficiency due to lowering Tafel slope values for HER (−38.96 mV dec−1) and OER (102.2 mV dec−1), surface oxidation layers due to Cu2+/Cu1+, good conductivity, charge transfer facility, and high electrocatalytic surface area. This study provides a plausible route to construct the C3N4 heterostructure Ti2O3/Ti3O5 with multiple interfaces, which is considered a good candidate for water splitting.

Reconciling of experimental and theoretical insights on the electroactive behavior of C/Ni nanoparticles with AuPt alloys for hydrogen evolution efficiency and Non-enzymatic sensor

We focused on a new feasible strategy for fabricating carbon-coated nickel (C/Ni) nanoparticles (NPs) with a AuPt alloy system using an integrated pulsed laser irradiation and ultrasonochemical process and provided insights on transferable electrocatalytic active surface states for HER and the selective detection of 1,4-benzenediol. The detailed physical characterization and electrochemical analyses revealed that the C/Ni–AuPt (0.12 mg/mL of AuPt) alloy showed exceptional electrocatalytic activities for HER in acidic media, with a low overpotential of 0.131 V at 10 mA/cm2, an exchange current density of 0.125 mA/cm2, a Tafel slope of 66 mV/dec, and a Tafel constant of 0.060 V. Additionally, an optimized C/Ni–AuPt electrocatalyst showed a broad dynamic linear response (50–250 μM) with high sensitivity (0.1134 μAμM−1cm−2) and low detection limit (0.185 μM) for sensing 1,4-benzenediol. Furthermore, an optimized C/Ni–AuPt alloys exhibited excellent electrochemical performance, long-term durability, and structural stability owing to the electronic effect of effective charge transfer from Au to Pt atoms, caused by a shift in the d-band center of Pt in AuPt alloys. The addition of C/Ni increased the active-sites of AuPt alloys because of the synergistic effect. Consequently, they provided abundant electrochemically active-surface areas necessary for the good dispersion of AuPt alloys. Alternatively, the strain effect was negligible in the C/Ni–AuPt structure. DFT calculations revealed that placing C/Ni NPs in direct contact with AuPt alloys displaces the d-band center of Au and Pt closer to the Fermi level, implying an increased activity of the electrocatalytic performance.

Surfactant-Free Monodispersed Pd Nanoparticles Template for Core-Shell Pd@PdPt Nanoparticles as Electrocatalyst towards Methanol Oxidation Reaction (MOR).

An eco-friendly two-step synthetic method for synthesizing Pd@PdPt/CNTs nanoparticles was introduced and studied for the methanol oxidation reaction. The Pd@PdPt alloy core-shell structure was synthesized by preparing a surfactant-free monodispersed Pd/CNTs precursor through the hydrolysis of tetrachloropalladate (II) ion ([PdCl4]2−) in the presence of carbon nanotubes (CNTs) and the subsequent hydrogen reduction and followed by a galvanic replacement reaction. This method opens up an eco-friendly, practical, and straightforward route for synthesizing monometallic or bimetallic nanoparticles with a clean surfactant-free electrocatalytic surface. It is quite promising for large-scale preparation. The Pd@PdPt/CNTs electrocatalyst demonstrated a high specific mass activity for methanol oxidation (400.2 mAmgPt−1) and excellent stability towards direct methanol oxidation compared to its monometallic counterparts.

Characterization of electrocatalytic proton reduction and surface adsorption of platinum nanoparticles supported by a polymeric stabilizer on an ITO electrode

Pt nanoparticles stabilized by a polymeric stabilizer of polyacrylic acid were stably adsorbed on an ITO electrode to work effectively and stably for electrocatalytic proton reduction.

Decoupled hydrogen evolution from water/seawater splitting by integrating ethylene glycol oxidation on PtRh0.02@Rh nanowires with Rh atom modification

PtRh nanowires with sub-monolayer of Rh atoms on the surface (PtRh0.02@Rh NWs) are fabricated and facilitate both hydrogen evolution reaction and ethylene glycol evolution reaction owing to the tensile strain and large electrocatalytic active surface area.

Electrocatalytic surface nanoionics with strained interfaced and colossal conductivity for enhancing durability and performance of solid oxide fuel cell

For an oxygen electrode in solid oxide fuel cells (SOFCs) consisting of mixed electrical and ionic conducting lanthanum strontium cobalt ferrite (LSCF), it degrades due to its low chemical stability and cation surface segregation. To mitigate such degradation, for the first time in the field of SOFCs, we demonstrate a conformal ultra-thin (∼10 nm) coating consisting of subjacent discrete nano-Pt capped with a superjacent conformal CoO x layer, applied on LSCF/SDC composite electrode, using atomic layer deposition (ALD). The coating layer reduces the cell series resistance by up to 40%, presents extraordinary stability with an intact morphology after 816 h operation. The superjacent CoO x surface nanoionics consists of randomly orientated but single-layered nanograins, with high-density intergranular and surface grain boundaries serving as the electrochemical reaction sites and facilitating mass transport. The ALD coating turns the original perovskite surface that is vulnerable to cation segregation and degradation into an embedded strained interface phase with enormous conductivity. The coating layer appears to suppress Sr outward diffusion and confines a 2 nm Sr-enriched interface layer between the coating layer and the LSCF backbone. The conductivity of the coating layer is estimated to be ∼1.27 × 10 4 S/cm and two orders magnitude higher than that of LSCF. • Conformal CoO x nanoionics with discrete Pt nano-particles on LSCF/SDC. • Heterogeneous CoO x /Pt reduces the cell series resistance by 40%. • CoO x /Pt ALD layer possesses extraordinary nanostructure stability over 816 h. • CoO x /Pt ALD layer suppresses Sr outward diffusion. • Conductivity of the ALD layer is two orders magnitude higher than that of LSCF.

Elaboration of a novel nanosensor using nanoparticles of α-Fe2O3 magnetic cores for the detection of metronidazole drug. Urine human and tap water

Metronidazole (MTZ) is a widely used antibiotic to treat infections caused by anaerobic bacteria, protozoa, and bacteroids such as trichromonosis and vaginosis. In this study, we present a simple strategy for constructing an electroanalysis platform for metronidazole in real samples. We prepared a modified carbon paste with α-Fe2O3 magnetic core nanoparticles to construct an α-Fe2O3@CPE electrochemical sensor. The surface morphology and composition of the sensor were evaluated using several methods, such as X-ray diffraction and scanning electron microscope. The average size of the α-Fe2O3 magnetic core nanoparticles was around 34.30 ​nm. Cyclic voltammetry, electrochemical impedance spectroscopy and chrono-coulometry were performed for the understanding of the electron transfer behavior on the electrocatalytic surface of α-Fe2O3@CPE and the unmodified electrode CPE. The resulting sensor demonstrates a very good shift of the Metronidazole reduction peak to a more positive potential (−0.57v vs Ag/AgCl) compared to the unmodified CPE electrode (−0.71v .vs Ag/AgCl). The Metronidazole peak reduction current Ipc varies linearly with metronidazole concentration in the range of 10-4 ​M to 0.8x10-6 ​M with a limit of detection and limit of quantification of 2.852x10-7 ​M and 9.509x10-7 ​M respectively. Exceeding the detection limits of several existing analytical methods. The proposed procedure has been successfully demonstrated on pharmaceutical tablets and real tap water and urine samples.

Enzymeless voltammetric sensor for simultaneous determination of parathion and paraoxon based on Nd-based metal-organic framework

The aim of this work is to fabricate a sensitive and novel enzymeless electrochemical sensor for the simultaneous determination of parathion and paraoxon using the Nd-UiO-66@MWCNT nanocomposite. For this purpose, Neodymium (Nd) was introduced into a Universitetet i Oslo (UiO-66) structure to construct Nd-UiO-66 and then, adding multi-walled carbon nanotubes to the Nd-UiO-66 to increase the electrocatalytic activity and surface area of the obtained composite. The Nd-UiO-66@MWCNT has numerous advantages like excellent conductivity, tunable texture, and large surface area and can be used as a distinctive structure for the construction of modified glassy carbon electrode (GCE) to enhance the charge-transfer and the efficiency of electrochemical sensors. This modified electrode showed sensitive and selective determination of paraoxon and parathion over the linear ranges of 0.7–100 and 1–120 nM, with detection limits of 0.04 and 0.07 nM, respectively. The proposed Nd-UiO-66@MWCNT/GCE sensor in this study can be applied in environmental and toxicological laboratories and field tests to detect parathion and paraoxon levels.

Engineering Electrochemical Surface for Efficient Carbon Dioxide Upgrade

AbstractElectrochemical CO2 conversion offers an attractive route for recycling CO2 with economic and environmental benefits, while the catalytic materials and electrode structures still require further improvements for scale‐up application. Electrocatalytic surface and near‐surface engineering (ESE) has great potential to advance CO2 reduction reactions (CO2RR) with improved activity, selectivity, energetic efficiency, stability, and reduced overpotentials. This review initially provides a panorama of ESE effects to give a clear perspective and leverage their advantages, including surface electronic effects, ensemble effects, strain effects, and local environment effects. Additionally, relevant in situ spectroscopic characterization techniques to detect, and theoretical computational approaches to reveal these ESE effects are presented. Typical ESE strategies are also summarized, e.g., in situ surface reconstruction, surface morphology control, surface modifications, etc. Rational manipulations of specific ESE approaches or combinations of them are critical to designing composite catalysts and electrodes, consequently promoting sustainable development and steadily increasing the prosperity of this field.

Laccase bioconjugate and multi-walled carbon nanotubes-based biosensor for bisphenol A analysis

Bisphenol A (BPA) is an endocrine disruptor compound that has been detected in aquatic ecosystems. In this work, the development of an electrochemical biosensor for BPA determination based on laccase from Trametes versicolor is reported. A bioconjugate was optimized to maximize the biosensor electrocatalytic activity and stability, which for the first time involved the synergistic effect of this specific enzyme (6.8 UmL−1), chitosan (5 mgmL−1) and the ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate in an optimum 5:5:2 (v/v/v) proportion. This bioconjugate was deposited onto a screen-printed carbon electrode previously modified with multi-walled carbon nanotubes (MWCNTs). Nanostructuration with MWCNTs enlarged the electrocatalytic activity and surface area, thus improving the biosensor performance. The BPA electrochemical reaction follows an EC mechanism at the optimum pH value of 5.0. Linearity up to 12 µM, a sensitivity of (6.59 ± 0.04) × 10-2 μAμM−1 and a detection limit of 8.4 ± 0.3 nM were obtained coupled with high reproducibility (relative standard deviations lower than 6%) and stability (87% of the initial response after one month). The developed biosensor was employed to the analysis of BPA in river water displaying appropriate accuracy (94.6–97.9%) and repeatability (3.1 to 6% relative standard deviations) proving its high potential applicability for in situ environmental analysis.

Enhancement of the electrocatalytic activity for the oxygen reduction reaction of boron-doped reduced graphene oxide via ultrasonic treatment

Commercial polymer electrolyte membrane fuel cells have relied on scares Platinum to catalyse the kinetically sluggish oxygen reduction reaction occurring at their anodes. Over the last decade organic materials, frequently based on graphitic structures have been demonstrated as promising alternative electrocatalysts to the noble metals. Researchers typically utilize ultrasonic treatment as part of the synthesis procedure to achieve homogeneous dispersion of graphitic carbon prior to. Herein we investigate the implications of the structural and compositional changes induced by the ultrasonication treatment on boron-doped reduced graphene oxide for oxygen reduction reaction. It is shown that ultrasonication pre-treatment prior to the boron doping and reduction of graphene oxide via hydrothermal process step leads to the increase of both substitutional B and electrocatalytic surface area, with associated reduction of average pore size diameter, leading to a significant improvement in the oxygen reduction reaction performance, with respect to the non-ultrasonicated material. It is proposed that the higher degree of substitutional doping of boron is a result of formation of the additional epoxy functionalities on graphitic planes, which act as a doping site for boric acid.

Modern applications of scanning electrochemical microscopy in the analysis of electrocatalytic surface reactions

Development of reaction-tailored electrocatalysts is becoming increasingly important as energy and environment are among key issues governing our sustainable future. Electrocatalysts are inherently optimized for application towards reactions of interest in renewable energy, such as those involved in water splitting and artificial photosynthesis, owing to its energy efficiency, simple fabrication, and ease of operation. In this view, it is important to secure logical design principles for the synthesis of electrocatalysts for various reactions of interest, and also understand their catalytic mechanisms in the respective reactions for improvements in further iterations. In this review, we introduce several key methods of scanning electrochemical microscopy (SECM) in its applications towards electrocatalysis. A brief history and a handful of seminal works in the SECM field is introduced in advancing the synthetic designs of electrocatalysts and elucidation of the operating mechanism. New developments in nano-sizing of the electrodes in attempts for improved spatial resolution of SECM is also introduced, and the application of nanoelectrodes towards the investigation of formerly inaccessible single catalytic entities is shared.

Electrochemical investigation of a tulsi-holy basil-crude plant extract on graphitized mesoporous carbon nanomaterial surface: Selective electrocatalytic activity of surface-confined rosmarinic acid for phenyl hydrazine-pollutant oxidation reaction

• A crude-plant extract was used for the preparation of a surface-confined redox system and electrocatalysis. • Selective electrochemical extraction of rosmarinic acid from Tulsi (Ocimum Sanctum)-Water Extract was occurred. • Rosmarinic acid-immobilized graphitized mesoporous carbon modified electrode was prepared. • Qualitative and quantitative electroanalysis of rosmarinic acid in a Tulsi Plant extract was demonstrated. • Selective electrocatalytic oxidation and flow injection analysis of Phenyl hydrazine were demonstrated. The mystery of > 2000 years of Hindu culture holy basil plant-Tulsi (Ocimum tenuiflorum)’s active ingredient for health benefit has been revealed by performing a blind cyclic voltammetric based electrochemical experiment (without pre-targeted chemicals) with a crude solution of the Tulsi-plant-water extract (TE) using a graphitized mesoporous carbon nanomaterial modified glassy carbon electrode (GCE/GMC) in pH 2 solution. The as-prepared chemically modified electrode was characterized using TEM, FTIR, Raman, UV–Vis, HPTLC, UPLC and with several control samples to identify the active molecular species trapped by GMC. It has been revealed that amongst various phytochemicals-ingredients, the rosmarinic acid (RA) in the TE-extract trapped selectively on the graphitic sites and showed an exceptionally efficient redox behavior at an apparent standard electrode potential, E o’ = 0.550 V vs Ag/AgCl with a peak-to-peak potential difference, ΔE p ∼ 0 V. A specific interaction between the π-electrons of the aromatic compound and sp 2 carbon of GMC is found to be an influencing parameter for the selective electrochemical micro-extraction of the RA from the TE (GMC@TE-RA). This electrochemical methodology helps for qualitative and quantitative analysis of the phytochemical, RA in the TE. The GMC@TE-RA is found to involve selective electrocatalytic oxidation of phenylhydrazine-pollutant in pH 2 KCl-HCl medium. Electrochemical impedance spectroscopic analysis of the modified electrode showed a superior electronic activity over the respective unmodified electrode. A scanning electrochemical microscopy (SECM) has been used to image the active site of the electrocatalytic surface. As a sustainable and green electrochemical approach, a highly selective electrocatalytic oxidation and flow injection analysis-based sensing of phenylhydrazine using the GCE/GMC@TE-RA has been demonstrated without any interference from hydrazine and other common electroactive chemicals and biochemicals.

Function of Doping Ru Element in the Hydrogen Evolution Reaction in Rare-Earth Transition-Metal Intermetallics.

Transition metal-based intermetallics are promising electrocatalysts for replacing the commercial Pt metal in the hydrogen evolution reaction (HER). In this work, RENi2 and RERu0.25Ni1.75 (RE = Pr, Tb, and Er) were synthesized and their electrocatalytic HER activities were explored. Among undoped compounds, PrNi2 exhibits the best performance and requires an overpotential of 55 mV, while partially replacing Ni with Ru element (PrRu0.25Ni1.75) can greatly reduce the overpotential to 20 mV at a current density of 10 mA/cm2. Such enhancement was recognized that belongs to their extrinsic property, and their intrinsic HER activities were similar after normalizing the electrocatalytic surface area. Further investigation on ScM2 and ScRu0.25M1.75 (M = Co and Ni) suggests that doping Ru element in ScCo2 will significantly enhance antibonding character around the Fermi level (EF) and weaken hydrogen adsorption energy. On the other hand, the antibonding population for ScNi2 and ScRu0.25Ni1.75 is similar at EF, which accounts for their close intrinsic HER activities.

Synthesis of ZnO nanoparticles on carbon graphite and its application as a highly efficient electrochemical nano-sensor for the detection of amoxicillin:analytical application: milk, human urine, and tap water

Amoxicillin is an antimicrobial of the penicillin class discovered in 1928. The objective of this paper is to construct a simple platform for electrocatalytic detection of amoxicillin using a ZnO@CPE nano-sensor constructed using simple and inexpensive processes using hydrothermal methods. Our results show that the constructed ZnO@CPE electrode exhibits excellent electrocatalytic activity compared to the unmodified electrode, with consistent, reproducible, and stable behavior. The electrochemical behavior of the amoxicillin oxidation reaction is diffusion controlled and fully reversible. The effect of the pH of the phosphate buffer solution on the antibacterial behavior of amoxicillin shows that the number of protons and electrons were equal. The morphology and chemical composition of the constructed nanoparticles were characterized by scanning electron microscope, transmission electron microscope, high-resolution transmission electron microscope, X-ray diffractometer, and infrared spectroscopy. Suggest the formation of zinc oxide nanocrystals on the carbon sheets with an order size of 22.957 nm. The diffusion coefficient and catalytic rate constant were 1.135 × 10–4 cm2/s and 8.314 × 103 mol.l−1/s, respectively. The proposed nano-sensor demonstrated a wide linearity range from 10–4 M to 10–6 M with LOD = 1.21 × 10–7 M and LOQ = 3.32 × 10–7 M according to the square-wave voltammetry method. The ZnO@CPE nano-sensor was examined for the detection of amoxicillin in real samples. Schematic concept of amoxicillin detection on the electrocatalytic surface of the nano-sensor fabricated with ZnO@CPE.