Oxide Electrodes Research Articles

Horseradish peroxidase enzyme/graphene oxide based electrochemical biosensor for detection of glutathione

Glutathione (GSH) is a tripeptide composed of three amino acids: cysteine, glycine, and glutamate. It is essential to many different living things as an antioxidant. Glutathione serves as a key biomarker and its detection is crucial for studying its levels in living bodies, providing insights into various diseases. In this work, we present the use of a highly sensitive electrochemical sensor to detect glutathione utilizing a graphene oxide modified Indium Tin Oxide (ITO) electrode immobilized with the enzyme horseradish peroxidase (HRP). The modified electrode was further characterized by Fourier transform infrared spectroscopy (FTIR) and spectrum showed that HRP was successfully immobilized onto GO. The electrochemical behavior of the modified ito was examined by cyclic voltammetry. Cyclic voltammetry demonstrated HRP/GO/ITO electrode has better electrocatalytic activity than bare ito in the oxidation of GSH in acetate buffer solution. The electrochemical sensor had a 1μM detection limit and a linear range of 10μM to 50 μM. The HRP/GO/ITO electrode resulted improved electrocatalytic properties, long-term stability, good repeatability and high sensitivity, and, along with a quick response to detect GSH. Additionally, GSH concentration in real sample was measured using the HRP/GO/ITO modified electrode.

Surface-engineered vertically-aligned ZnO nanorod for sensitive non-enzymatic electrochemical monitoring of cholesterol

Developing highly sensitive and selective non-enzymatic electrochemical biosensors for disease biomarker detection has become challenging in healthcare applications. However, advances in material science are opening new avenues for creating more dependable biosensing technologies. In this context, the present work introduces a novel approach by engineering a hybrid structure of zinc oxide nanorod (ZnO NR) modified with iron oxide nanoparticle (Fe2O3 NP) on an FTO electrode. This Fe2O3 NP-ZnO NR hybrid material functions as a nanozyme, facilitating the catalysis of cholesterol and enabling the direct transfer of electrons to the fluorine-doped tin oxide (FTO) electrode, limiting the need for costly and traditional enzymes in the detection process. This innovative non-enzymatic cholesterol biosensor showcases remarkable sensitivity, registering at 642.8 μA/mMcm2 within a linear response range of up to 9.0 mM. It also exhibits a low detection limit (LOD) of ∼12.4 μM, ensuring its capability to detect minimal concentrations of cholesterol accurately. Moreover, the developed biosensor displays exceptional selectivity by effectively distinguishing cholesterol molecules from other interfering biological species, while exhibiting outstanding stability and reproducibility. Our findings indicate that the Fe2O3 NP-ZnO NR hybrid nanostructure on the FTO electrode holds promise for enhancing biosensor stability. Furthermore, the present device fabrication platform offers versatility, as it can be adapted with various enzymes or modified with different metal oxides, potentially broadening its applicability in a wide range of biomarkers detection.

Unveiling Intercalation Chemistry via Interference-Free Characterization Toward Advanced Aqueous Zinc/Vanadium Pentoxide Batteries.

Aqueous Zn/V2O5 batteries are featured for high safety, low cost, and environmental compatibility. However, complex electrode components in real batteries impede the fundamental understanding of phase transition processes and intercalation chemistry. Here, model batteries based on V2O5 film electrodes which show similar electrochemical behaviors as the real ones are built. Advanced surface science characterizations of the film electrodes allow to identify intercalation trajectories of Zn2+, H2O, and H+ during V2O5 phase transition processes. Protons serve as the vanguard of intercalated species, facilitating the subsequent intercalation of Zn2+ and H2O. The increase of capacity in the activation process is mainly due to the transition from V2O5 to more active V2O5·nH2O structure caused by the partial irreversible deintercalation of H2O rather than the increase of active sites induced by the grain refinement of electrode materials. Eventually, accumulation of Zn species within the oxide electrode results in the formation of inactive (Zn3(OH)2V2O7·2H2O) structure. The established intercalation chemistry helps to design high-performance electrode materials.

Sensitive photoelectrochemical detection of Cr(Ⅵ) based on the suppression of background photocurrent

A photoelectrochemical (PEC) sensor based on a BiVO4 semiconductor and gold nanoparticles (AuNPs) was successfully prepared for the sensitive detection of Cr(Ⅵ) ions. The calcination temperature was found to be very important for the PEC properties of BiVO4. The BiVO4-modified indium tin oxide electrode (ITO/BiVO4) calcined at 300 °C generated a low cathodic photocurrent response under light irradiation. BiVO4/AuNPs materials were coupled via electrostatic adsorption to enhance the photoelectric conversion performance of BiVO4. The use of self-assembled monolayers (SAMs) to modify electrodes reduce the background current. The developed ITO/BiVO4/AuNPs/L-Cys PEC sensor was used to detect of Cr(VI). The Cr(Ⅵ) ion concentrations showed a good linearity between 10 pM and 1 μM with a detection limit of 9.1 pM (S/N = 3). The prepared PEC sensor exhibited high sensitivity, a wide linear range, and good selectivity. This work provides a promising platform for the analytical detection of heavy metal ions.

Innovative voltammetric techniques for bumadizone analysis in pharmaceutical and biological samples: emphasizing green, white, and blue analytical approaches

There are no documented electroanalytical methods for quantifying the anti-inflammatory drug bumadizone (BUM) in pharmaceutical or biological matrices. So, a new voltammetric method was developed to determine BUM at nano concentrations in pharmaceutical forms, in the presence of its alkaline degradant, and in biological fluids. Five electrodes were tested, including three nano-reduced graphene oxide (nRGO) electrodes (5%, 15%, and 20%), a carbon paste electrode (CPE), and a 10% nRGO-modified CPE. The 10% nRGO-modified electrode showed the best performance, offering high selectivity and low detection limits, with good linearity in the concentration range of 0.9 × 102 to 15 × 102 ng mL−1. Differential pulse voltammetry successfully applied this electrode for BUM determination in various samples, achieving excellent recovery without preliminary separation. The method was validated according to ICH guidelines and compared favorably to the reference method. Its environmental impact was assessed using AGREE and Eco-scale metrics in addition to the RGB algorithm, showing superior greenness and whiteness profiles due to safer solvents and lower energy consumption, along with high practical effectiveness using the BAGI metric.

Efficient electrochemical degradation of ranitidine by a novel Bi-coated titanium oxide electrode: Performance and mechanism

Ranitidine (RAN) is a commonly prescribed medication that poses ecological risks due to its potential to transform into the carcinogenic byproduct N-nitrosodimethylamine (NDMA) in the environment. Herein, we synthesized a novel bismuth-coated titanium oxide (Bi-Ti4O7) electrode using a straightforward coating method and evaluated its effectiveness in the electrochemical oxidation of RAN. The Bi-Ti4O7 electrode achieved a degradation efficiency of 90.41 % for an initial RAN concentration of 10 mg/L within 120 min, greatly outperforming the pristine Ti4O7 electrode. The incorporation of Bi enhances the oxygen vacancies and charge transfer characteristics, facilitating direct electron transfer between RAN and the Bi-Ti4O7 electrode. The potential degradation pathways of RAN by the Bi-Ti4O7 electrode included C–S bond cleavage, C–N bond cleavage, and electrophilic oxidation. No NDMA was generated during the oxidation process, and the toxicity of RAN oxidation intermediates was greatly reduced. The Bi-Ti4O7 electrode demonstrated excellent stability, maintaining over 90 % degradation efficiency across 30 cycles, and showed wide applicability across different pH levels and wastewater types with negligible Bi ion release (0.148 µg/L). These results underscore the potential of Bi-Ti4O7 as an effective and sustainable solution for RAN-polluted wastewater treatment.

Controlled synthesis of Sn doped Cu–Ni3S2 on Ni foam as efficient electrocatalyst for urea oxidation reaction and oxygen evolution reaction

Hydrogen production technology by urea-assisted electrocatalytic water decomposition has become one of the important means to alleviate carbon emissions and water pollution. In this paper, we first doped Sn and Cu element into the Ni3S2 material by hydrothermal method on the Ni foam support. This Cu–Sn–Ni3S2 material exhibits superior urea (potential of 1.42 V at 100 mA cm−2) and water oxidation (potential of 1.63 V at 100 mA cm−2) properties, which is one of the best electrochemical performance reported up to now. Analysis of experiment demonstrate that the increase in catalytic performance is assigned to faster charge transfer, more exposure of reaction centres and smaller resistance owing to doping of Sn and Cu. Density functional theory (DFT) analysis demonstrates that introduction of Sn and Cu increases the adsorption energy of urea and improves the conductivity of the Cu–Sn–Ni3S2 material, and the co-doping of the two changes the electron state density of the active site, thereby promoting the catalytic performance. This work provides insights into the development of efficient bifunctional electrodes for urea oxidation and oxygen evolution reaction through doping strategies.

Ultrafast Sodium–Ion Batteries Based on Vanadium Oxide and Laser-Scribed Graphene Electrodes

Ultrafast Sodium–Ion Batteries Based on Vanadium Oxide and Laser-Scribed Graphene Electrodes

Molecular O2 Dimers and Lattice Instability in a Perovskite Electrocatalyst.

Structural degradation of oxide electrodes during the electrocatalytic oxygen evolution reaction (OER) is a major challenge in water electrolysis. Although the OER is known to induce changes in the surface layer, little is known about its effect on the bulk of the electrocatalyst and its overall phase stability. Here, we show that under OER conditions, a highly active SrCoO3-x electrocatalyst develops bulk lattice instability, which results in the formation of molecular O2 dimers inside the bulk and nanoscale amorphization induced via chemo-mechanical coupling. Using high-resolution resonant inelastic X-ray scattering and first-principles calculations, we unveil the potential-dependent evolution of lattice oxygen inside the perovskite and demonstrate that O2 dimers are stable in a densely packed crystal lattice, thus challenging the assumption that O2 dimers require sufficient interatomic spacing. We also show that the energy cost of local atomic rearrangements in SrCoO3-x becomes very low under the OER conditions, leading to an unusual amorphization under intercalation-induced stress. As a result, we propose that the amorphization energy can be calculated from the first principles and can be used to assess the stability of electrocatalysts. Our study demonstrates that extreme oxidation of electrocatalysts under OER can intrinsically destabilize the lattice and result in bulk anion redox and disorder, suggesting why some oxide materials are unstable and develop a thick amorphous layer under water electrolysis conditions.

Facile Fabrication of Bio-Nanohybrid Electrode with Guanine/Cytosine-Modified Electrochemically Reduced Graphene Oxide Electrode and Its Application in Doxorubicin Analysis

Graphene, known for its outstanding physical and chemical properties, is widely used in various fields, including electronics and biomedicine. Reduced graphene oxide (rGO) is preferred for electrochemical applications due to its enhanced water solubility and dispersion. Electrochemically reduced graphene oxide (ErGO) is particularly advantageous as it can be prepared under mild conditions and simplifies sensor fabrication; however, ErGO-based electrochemical sensors often lack specificity. Bioreceptors like proteins, enzymes, and DNA/RNA aptamers are incorporated to provide high specificity. This study introduces a guanine (G)/cytosine (C)-modified ErGO electrode (G/C@ErGO-GCE) for the sensitive electrochemical detection of doxorubicin (DOX) with good selectivity. The G/C mixture acts as a bioreceptor and is anchored on the ErGO-GCE surface via π-π interactions. The G/C@ErGO-GCE was characterized using scanning electron microscopy, contact angle measurement, Raman spectroscopy, and electrochemical methods. The sensor demonstrated excellent dynamic range (DPV: 10 nM to 1 µM, CA: 30 nM to 1.3 µM), sensitivity (DPV: 2.17 µA/µM, CA: 6.79 µA/µM), limit of detection (DPV: 84 nM, CA: 34 nM), and selectivity for DOX detection, highlighting its potential for biomedical applications and pharmacokinetic studies.

Dual-capable spinel cobalt oxide nanoparticles for electrocatalytic oxygen evolution and water contaminant removal.

This study investigates the synthesis and electrocatalytic performance of cobalt oxide (Co3O4) nanoparticles for the oxygen evolution reaction (OER) and their role in water treatment as contaminant removal agents. Cobalt oxide nanoparticles are recognized as promising materials in electrocatalysis due to their tunable properties and nanoscale engineering potential. Here, fine cobalt oxide nanoparticles are synthesized using the sol-gel method followed by various sintering temperatures to achieve precise control over surface morphology, size, and shape. Characterization via high-resolution scanning electron microscopy (HRSEM) and high-resolution transmission electron microscopy (HRTEM) elucidates the impact of sintering temperature on nanoparticle properties. Thin film electrodes of cobalt oxide are fabricated using the doctor blade method and evaluated using linear sweep voltammetry (LSV) and electrochemical impedance spectroscopy (EIS). Among the tested sintering temperatures, cobalt oxide electrodes sintered at 600°C exhibit superior catalytic activity, demonstrating an overpotential of 258mV (vs RHE) at 10mAcm-2 current density and a Tafel slope of 17.33mV dec-1. Furthermore, these electrodes demonstrate excellent stability, maintaining OER performance for 10h in 1M NaOH electrolyte. Additionally, the role of cobalt oxide nanoparticles in water treatment is explored using inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental results reveal that lower sintering temperatures enhance the electrocatalytic properties of cobalt oxide nanoparticles, highlighting their potential contribution to sustainable energy and water treatment technologies. This work underscores the significance of cobalt oxide nanoparticles as dual-functional materials for advancing electrocatalysis and water purification applications, thus paving the way for the development of efficient and environmentally friendly technologies.

The Review of Treatment of Copper Ion in Wastewater and Comparison Between Four Treatment

This paper presents a comprehensive review of various methods used to remove copper ions from wastewater, highlighting their efficiency and feasibility. The main focus is on adsorption, ion flotation, membrane-based techniques, and electrochemical cells, with a particular emphasis on innovative approaches like the use of graphene oxide electrodes. The comparison and analysis section assesses each method’s removal efficiency, operational challenges, and costs, providing a critical perspective on their practical application in industrial settings.

First approach of fractals nickel-copper dendrites on stainless steel electrodes for ammonia oxidation to nitrogen monitored in operando by differential electrochemical mass spectroscopy

Fractal nickel-copper dendrites were synthesized by electrochemical deposition (ECD) on a stainless steel electrode (SS/NiCu). The electrode surface was characterized using Field Emission Scanning Electron Microscopy (FE-SEM), X-ray diffractometry (XRD), and Raman spectroscopy. The Ni-Cu molar ratio and the time applied in the ECD method were studied, revealing that both are critical factors in modifying and controlling the surface morphology. The SS/NiCu electrodes show a higher density current response when exposed to ammonium hydroxide, reaching a limiting current density at concentrations above 0.050 M NH4OH. Ammonia oxidation reaction (AOR) was monitored in operando using differential electrochemical mass spectroscopy (DEMS). When a bias potential over +1.50 V (vs. RHE) was applied, the evolution of oxygen and NO was observed. However, N2 was the only oxidation product at a constant potential below +1.50 V (vs. RHE). Oxygen (O2) evolution was the main competitive reaction during the AOR. The results show that products are strongly dependent on the electrochemical perturbation applied. The study demonstrated that the SS/NiCu electrodes are suitable for AOR to N2 in high alkaline conditions.

Assessment of Ti, Ir, Ta and Ru influence on mixed metal oxide electrodes for photoelectrochemical generation of persulfate: Impact on sulfamethoxazole degradation

The presence of persulfate (S2O82−) in decontamination processes favors the oxidation of organic pollutants due to its strong oxidation power. In this research we study the photoelectrochemical generation of persulfate using five mixed metal oxides electrodes (MMO) with different compositions and its effect on the degradation of sulfamethoxazole antibiotic (SMX) by photoelectrocatalysis (PEC) and electro-oxidation (EO).By PEC, all anodes generated a higher concentration of S2O82− than those not exposed to light. The high S2O82−concentration obtained by PEC was 0.150 mM using MMO[Ti/Ir/Ta] in a solution with Na2SO4 100 mM applying a current density of 2 mA/cm2. On the other hand, the maximum concentration obtained was 0.250 mM at 30 min of electrolysis for MMO[Ti/Ir/Ta] using Na2SO4 50 mM and applying current density of 5 mA/cm2. S2O82−production by EO was between 0.005 and 0.089 mM. It is observed that MMO based in Ta2O5 showed the best S2O82− production.The effect of S2O82− electro-generation (using the anode with the highest and the anode with the lowest S2O82− production) on the degradation of sulfamethoxazole by PEC and EO was studied using the experimental conditions with the best production of this oxidant. MMO[Ti/Ir/Ta] and MMO[Ti/Ru] were used as anodes, and it was observed that by PEC, 100% of SMX was degraded after 30 min of electrolysis using MMO[Ti/Ir/Ta] and 60 min using MMO[Ti/Ru]. By EO, the degradation of SMX was partial, demonstrating that the electrophotocatalytic effect favors the generation of S2O82−, enhancing the degradation of SMX at short electrolysis times.

The electrocatalytic degradation of 1,4-dioxane by Co-Bi/GAC particle electrode.

Efficient degradation of industrial organic wastewater has become a significant environmental concern. Electrochemical oxidation technology is promising due to its high catalytic degradation ability. In this study, Co-Bi/GAC particle electrodes were prepared and characterized for degradation of 1,4-dioxane. The electrochemical process parameters were optimized by response surface methodology (RSM), and the influence of water quality factors on the removal rate of 1,4-dioxane was investigated. The results showed that the main influencing factors were the Co/Bi mass ratio and calcination temperature. The carrier metals, Co and Bi, existed mainly on the GAC surface as Co3O4 and Bi2O3. The removal of 1,4-dioxane was predominantly achieved through the synergistic reaction of electrode adsorption, anodic oxidation, and particle electrode oxidation, with ·OH playing a significant role as the main active free radical. Furthermore, the particle electrode was demonstrated in different acid-base conditions (pH = 3, 5, 7, 9, and 11). However, high concentrations of Cl- and NO3- hindered the degradation process, potentially participating in competitive reactions. Despite this, the particle electrode exhibited good stability after five cycles. The results provide a new perspective for constructing efficient and stable three-dimensional (3D) electrocatalytic particle electrodes to remove complex industrial wastewater.

Nanochannel-confined platinum nanostructure for enhancement of luminol-dissolved oxygen electrochemiluminescence coupled with gated aptasensor for sensitive detection of carcinoembryonic antigen

Rapid and precise detection of tumor biomarkers in serum is of great significance for early diagnosis, treatment assessment, and recurrence monitoring of cancers. The fabrication of user-friendly electrochemiluminescence (ECL) aptasensors with effective signal amplification is highly desirable. In this study, an ECL aptasensor was developed with luminol-based ternary ECL platform using dissolved oxygen as endogenous co-reactant and nanochannel-confined platinum nanoparticles (PtNPs) as co-reactant promoter, which can realize highly sensitive detection of the tumor biomarker, carcinoembryonic antigen (CEA). On the cost-effective indium tin oxide (ITO) electrode, amino-modified vertically-ordered mesoporous silica film (NH2-VMSF) was easily grown to form high-density nanochannel array with ultrasmall nanochannels. PtNPs were then in-situ synthesized within the nanochannels via electrodeposition. Ternary ECL system was successfully fabricated as confined PtNPs can catalyze the electroreduction of dissolved oxygen at negative potentials as well as electrochemical oxidation of luminol, enhancing the ECL signal of luminol. The recognitive aptamer (Apt) was covalently immobilized on the outer surface of NH2-VMSF, resulting in the fabrication of an aptasensor. In presence of CEA, a decreased ECL signal was obtained as the formed complex on the recognition interface hindered the diffusion of ECL emitter to the supporting electrode. Based on this signal turn-off mode, sensitive detection of CEA was achieved ranged from 10 fg mL−1 to 100 ng mL−1, with a low detection limit (DL, 0.4 fg mL−1). The aptasensor displayed high selectivity and good reproducibility. The nanochannel-based aptasensor and ternary ECL system demonstrates great potential in convenient and sensitive detection of cancer biomarker.

Surface and Grain Boundary Coating for Stabilizing LiNi0.8Mn0.1Co0.1O2 Based Electrodes.

The widespread use of high-capacity Ni-rich layered oxides such as LiNi0.8Mn0.1Co0.1O2 (NMC811), in lithium-ion batteries is hindered due to practical capacity loss and reduced working voltage during operation. Aging leads to defective NMC811 particles, affecting electrochemical performance. Surface modification offers a promising approach to improve cycle life. Here, we introduce an amorphous lithium titanate (LTO) coating via atomic layer deposition (ALD), not only covering NMC811 surfaces but also penetrating cavities and grain boundaries. As NMC811 electrodes suffer from low structural stability during charge and discharge, We combined electrochemistry, operando X-ray diffraction (XRD), and dilatometry to understand structural changes and the coating protective effects. XRD reveals significant structural evolution during delithiation for uncoated NMC811. The highly reversible phase change in coated NMC811 highlights enhanced bulk structure stability. The LTO coating retards NMC811 degradation, boosting capacity retention from 86 % to 93 % after 140 cycles. This study underscores the importance of grain boundary engineering for Ni-rich layered oxide electrode stability and the interplay of chemical and mechanical factors in battery aging.

Application of metal oxide/porous carbon nanocomposites in electrochemical capacitors: A review

In the past decade, electrochemical capacitors (ECs) have emerged as innovative energy storage devices, attracting considerable interest from both industrial and academic sectors due to their prolonged cyclic stability and impressive power density. Recently, there has been a focus on advancing high-performance ECs by developing electrode material composed of metal oxide incorporated with porous carbon. Integrating metal oxides into a porous carbon structure enhances capacitance, charge storage, and cyclic stability. Furthermore, the porous structure inherent in carbon materials offers efficient ion diffusion and large surface area, thereby augmenting the overall effectiveness of the nanocomposites. Efficient electron and ion transport within the electrode's bulk is achieved through the interaction between electrodes and electrolytes occurring at the electrode-electrolyte interface, subsequently increasing the capacitance. This paper summarizes the latest developments in ECs, focusing on key performance metrics such as cyclic stability and capacitance. It also summarizes the recent advancements made in electrode materials, emphasizing the utilization of sustainable feedstocks. As the research landscape shifts towards more environmentally friendly solutions, the incorporation bio-materials into electrode design has gained significant attention. It particularly highlights underlying mechanisms governing the performance of metal oxides/porous carbon nanocomposites in ECs and outlines future research directions aimed at maximizing their potential for next-generation energy storage devices. Additionally, the paper delves into the possibilities and challenges associated with the preparation, and optimization of the structure of metal oxide electrodes incorporating porous carbon to improve energy storage performance in ECs.

Gallium Nitride Electrodeposition at Indium Tin Oxide and Fluorine Tin Oxide Electrodes in Ammonium Nitrate and Gallium Nitrate Aqueous Solution

The potential of gallium nitride thin films in semiconductor technology and devices has garnered interest. This study aims to develop an effective GaN electrodeposition technique that will function on both Earth and microgravity situations and may be applied to any kind of needed application, such as in photovoltaic devices. To determine the optimal electrodeposition conditions, e.g. applied potential, cyclic voltammetry (CV) was done on a boron-doped diamond electrode at 0.01 mV/s potential scan rate and at 0.8 V vs. Ag/AgCl (Saturated KCl) constant applied potential. In the CV study, a well-defined peak formed at -1.75 V vs. Ag/AgCl (Saturated KCl). To start examining all the features of the electrodeposition of a thin film on Indium Tin Oxide (ITO) and Fluorine Tin Oxide (FTO) Electrodes, chronoamperometry (CA) measurements were done at different time scales, ranging from 3600s to 14400s and at a constant applied potential of -1.7 V vs. Ag/AgCl (Saturated KCl). The characterization methods used to examine the materials' topography, elemental contrast, crystal structure, and electrodeposition weight percentages included scanning electron microscopy (SEM), X-ray diffraction (XRD), and energy dispersive spectroscopy (EDS). Longer electrodeposition times produced the best grain formation, promoting dendritic structure at the electrode surface. Furthermore, the optimal weight electrodeposition percentage of Ga and N was 10% and 35 % at 3600s, respectively, although the electrodeposited electrode surface was heterogeneous. The surface topographies at 3600s showed less grains definition and dendritic structures. At higher electrodeposition times, e.g. 14400s, more grain definitions and dendritic structures were found. For the 3600s electrodeposition time, XRD peaks were found at 33o, 37o and 46o, which are characteristics of GaN wurtzite structure according to literature.

Ambient Deposition of Single Atoms for Enhancement of Nanostructured Metal Oxide Electrode Catalytic Performance

Single-atom decoration represents cutting-edge technology for enhancing heterogeneous catalysis by utilizing the unique capabilities of catalysts at the atomic level. However, the high surface energy of single atoms often causes them to aggregate, forming nanoparticles [1]. To address this challenge, we first modify the surface structure by synthesizing nanostructured support layers, such as TiO2 nanotubes, TiO2 nanosheets, and NiO nanosponge. Especially TiO2 nanotubes and NiO nanosponge pose relevant support layers due to their favorable attributes, including a high surface-to-volume ratio, abundance, and excellent chemical stability, while TiO2 nanosheets serve as model system. Vertically aligned, well-ordered, self-organized oxide nanostructures can be conveniently fabricated through anodization, allowing precise control over the geometry of the nanotubes and nanopores [2,3]. Well-defined atomic-scale defects on the surface of the supports are generated to immobilize single-atom co-catalysts. Therefore, defect engineering techniques typically require high-temperature thermal reduction. We present more gentle defect-engineering approaches, including room-temperature sonochemical treatment or UV-light irradiation. By combining these approaches, we are able to effectively trap Pt and Ir single atoms.We present a direct method utilizing UV-light radiation to induce point defects, specifically Ti3+ and oxygen vacancies (VO) onto the surface of TiO2 nanosheets and efficiently decorate them with Pt single atoms [4]. Our findings demonstrate that sonochemically treated TiO2 nanotubes provide a remarkable substrate for single-atom decoration from dilute solutions, resulting in promising performance in H2 evolution catalysis and renewable energy conversion. Additionally, the role of V single-atom decoration in ultrasonic treatment of support materials is investigated.Thermal annealing in a reductive atmosphere induces the formation of numerous defects, facilitating the anchoring of single Ir atoms onto the surface of annealed NiO nanostructures. Additionally, the novel ultrasound-driven method stabilizes these Ir atoms within the porous structure. By employing both approaches, we effectively trap Ir single atoms, thereby enhancing the efficiency of the oxygen evolution reaction in electrocatalysis [5].The characterization of the electrodes is conducted using microscopy techniques (FESEM, TEM, and HAADF-STEM) and spectroscopy (XPS and ToF-SIMS) [6]. Gas chromatography is employed to evaluate the H2 photocatalytic performance of TiO2 electrodes, while linear sweep voltammetry is utilized to assess the H2 and O2 electrochemical activity of NiO electrodes [5]. Our findings highlight the significant enhancement of photo- and electrocatalytic efficiency of nanostructured oxide electrodes modified with highly stable single-atom co-catalysts by gentle treatments.