Oxide Composites Research Articles

Light-Driven Electrochemical Biosensing with DNA Origami-Assisted Hybrid Nanoantenna for Fumonisin B1 Monitoring.

The electrochemical detection of biosensors is largely governed by the changes in physical properties of redox probes, which are susceptible to electrode substrate effects, inhibiting sensor sensitivity. In this work, a light-driven electrochemical biosensor based on a hybrid nanoantenna was developed for the sensitive detection of fumonisin B1 (FB1). The hybrid nanoantenna sensing interface was constructed by coupling CdSe quantum dots (QDs)-DNA nanowire and graphdiyne oxide composites loaded with methylene blue and gold nanorods (GDYO-MB-Au NRs) using a tetrahedral DNA nanostructure, which acted as a light-driven unit and an amplification unit, respectively. The hybrid nanoantenna with light-driven properties facilitated the alteration in the chemical properties of MB at the sensing interface; that is, MB was degraded under light illumination. The stripping of the CdSe QDs-DNA nanowire triggered by the binding of FB1 could degrade the light-driven capability, thereby improving the electrochemical signal through depressing MB degradation. Taking advantage of the photodegradation of MB by the hybrid nanoantenna, the developed biosensor reduced the background signal and increased the detection sensitivity. The developed biosensor exhibited a linear detection range from 0.5 fg mL-1 to 10 pg mL-1 and a detection limit down to 0.45 fg mL-1. This strategy shows great promise for the fabrication of highly sensitive electrochemical biosensors.

Electrochemical sensing platform using reduced graphene oxide and Sn MOF-derived hollow cubic composites for sensitive detection of catechol in environmental water samples

Catechol, a polyphenolic molecule and significant organic chemical intermediate, is a highly dangerous environmental contaminant due to its unpredictable nature and potential harm to both humans and the environment. This study presents the development of Sn MOF@rGO-650, identified as a hollow cube by SEM and TEM, created by carbonizing rGO on the surface of Sn MOF after in situ encapsulation. The Sn MOF@rGO-650 modified glassy carbon electrode was successfully constructed for the electrochemical detection of catechol. Under optimal conditions, the sensor exhibited a detection limit of 33 nM, a linear range of 0.20 μM–28 μM, and good long-term stability and reproducibility. This work proves for the first time that Sn MOF@rGO-650 composites can effectively detect catechol in real environmental water samples, achieving recoveries between 95.7 % and 104.8 %, and is validated in UV spectroscopy, which highlights its potential for practical applications.

Effect of transition metal (M=Cr, Mn, Fe, Co) doping on catalytic combustion of chlorobenzene over Ce − Y composite oxide

Transition metal (Cr, Mn, Fe, Co)-doped CeYOx catalysts were prepared by a co-precipitation method and applied for chlorobenzene elimination. Metal doping caused significant changes in physical properties and chemical environment of CeY solid solution. Intrinsic activity of metals and their interaction with CeY significantly improved the redox performance and oxygen mobility, thus enhancing the catalytic activity and chlorine poisoning resistance. The enhanced concentration and mobility of reactive oxygen can effectively control chlorinated by-products. MnCeYOx can achieve 90 % chlorobenzene conversion at 235 °C, attributing to the promotion of the redox dynamic cycle by the enhanced mobility of active oxygen.

The lightweight titanium dioxide/reduced graphene oxide composites prepared by hydrothermal method for microwave absorption

To solve electromagnetic pollution, microwave absorption materials with high performance have gained attention. Manipulating the impedance matching is an effective strategy to obtain the outstanding electromagnetic wave absorption material. In this work, a series of titanium dioxide/reduced graphene oxide (TiO2/RGO) composites were prepared by the hydrothermal method for microwave absorption. The relationship between the microstructure and microwave absorption performance of the composite was analyzed in detail. The impedance matching and attenuation ability of TiO2/RGO composites could be precisely manipulated by regulating the titanium dioxide content. The reflection loss and effective absorption bandwidth of the TiO2/RGO composite could reach −46 dB and 3.36 GHz (1.9 mm), respectively. Thus, the lightweight TiO2/RGO composite has the potential application in microwave absorption.

Conformal TiO2 Aerogel-Like Films by Plasma Deposition: from Omniphobic Antireflective Coatings to Perovskite Solar Cell Photoelectrodes.

The ability to control the porosity of thin oxide films is a key factor determining their properties. Despite the abundance of dry processes for synthesizing oxide porous layers, a high porosity range is typically achieved by spin-coating-based wet chemical methods. Besides, special techniques such as supercritical drying are required to replace the pore liquid with air while maintaining the porous network. In this study, we propose a new method for the fabrication of ultraporous titanium dioxide thin films at room or mild temperatures (T ≤ 120 °C) by a sequential process involving plasma deposition and etching. These films are conformal to the substrate topography even for high-aspect-ratio substrates and show percolated porosity values above 85% that are comparable to those of advanced aerogels. The films deposited at room temperature are amorphous. However, they become partly crystalline at slightly higher temperatures, presenting a distribution of anatase clusters embedded in the sponge-like open porous structure. Surprisingly, the porous structure remains after annealing the films at 450 °C in air, which increases the fraction of embedded anatase nanocrystals. The films are antireflective, omniphobic, and photoactive, becoming superhydrophilic when subjected to ultraviolet light irradiation. The supported, percolated, and nanoporous structure can be used as an electron-conducting electrode in perovskite solar cells. The properties of the cells depend on the aerogel-like film thickness, which reaches efficiencies close to those of commercial mesoporous anatase electrodes. This generic solvent-free synthesis is scalable and applicable to ultrahigh porous conformal oxides of different compositions, with potential applications in photonics, optoelectronics, energy storage, and controlled wetting.

Bulk graphene-based composites with artificial nacre-like laminated structure: Microstructure and mechanical properties

In this study, the bulk Cu/reduced graphene oxide (Cu/rGO) composites featuring an artificial nacre-like laminated structure were successfully fabricated using spark plasma sintering (SPS), and the microstructure and mechanical properties of the resulting composites were investigated. The Cu/rGO composites demonstrated a distinct laminated structure, and their relative densities increase with Cu addition. Moreover, the presence of trace amounts of in-situ interfacial reaction products (CuO and CuO2,) were observed to enhance the adhesive strength at the Cu-rGO interface. Mechanical testing of the composites showed notable improvements in both compressive strength and ductility compared to a bulk monolithic rGO sample. Specifically, the bulk rGO composites with a 35.05 wt% addition of Cu displayed an enhancement of ∼67 % in compressive strength and ∼19 % in ductility relative to the pure rGO sample. These improvements are attributed to synergetic strengthening and toughening mechanisms within the rGO composites. The enhanced strength and ductility of the Cu/rGO composites significantly boost their wear resistance. This research not only demonstrates the effectiveness of incorporating Cu into rGO matrices but also suggests a promising avenue for the development of novel bulk rGO composites with engineered laminated structures.

Spinel-structured catalyst formed by Fe, Cu, and Co composites for efficient toluene oxidation

Due to its distinctive structure and properties, MFe2O4 has been extensively investigated in catalytic oxidation. In this study, we synthesized a ternary metal composite Fe-based spinel catalyst using the sol-gel method for toluene oxidation. The catalytic performance assessments showed that the catalytic performance of Cu0.7Co0.3Fe2O4 (T90 = 262 °C, 100,000 mL·g−1·h−1) was superior to that of CuFe2O4 (T90 = 270 °C) and CoFe2O4 (T90 = 310 °C), compared to binary metal spinel catalysts. The characterization results indicate that the strong interactions among Cu, Co, and Fe in the ternary metal composite structure increased the content of oxygen vacancy at lower temperatures, thereby increasing the content of surface reactive oxygen species and improving catalytic performance. This study highlights the potential application of Fe-based spinel structures to develop more efficient spinel catalysts.

One-step formation of synergistic ZnO/SnO2 composite nanostructures derived from annealing of crystalline ZnSn(OH)6 nanocubes for enhanced catalytic degradation of organic pollutants

Binary metal oxides/hydroxides derived primary metal oxide composites have a pivotal role in diverse applications because of the beneficial interfacial contact, good synergism, high porous nature, and high stability. The current work deals with the derived ZnO/SnO2 composite nanostructures from post-annealing crystalline ZnSn(OH)6 (ZTO-RT) nanocubes, initially synthesized via a single-step hydrothermal synthesis method. First, the pristine ZTO-RT is synthesized @ 180 °C in a hydrothermal autoclave. Further, the transformation of ZTO-RT to ZnO/SnO2 composite nanostructures is performed at two different annealing temperatures of 500 °C (ZTO-DV-500) and 750 °C (ZTO-DV-750) in the vacuum. The respective samples' physical characterization was studied and compared using various analytical techniques. The X-ray diffraction analysis affirms the amorphous nature of ZTO-DV-500 and the poly-crystalline nature of ZTO-DV-750. The nanocube morphologies of the samples are retained even at high-temperature sintering. The existence of metal-oxygen bonds on the surface of the ZnO/SnO2 composite is sustained by X-ray photoelectron spectroscopy. ZTO-DV-750 has larger pores (pore volume - 0.091 cm3 g−1) than the ZTO-DV-500 (0.051 cm3 g−1). In the presence of NaBH4 aqueous solution, the enhanced rhodamine B dye degradations of ZTO-DV-750 are observed. At low RhB concentrations (5 mg L−1), the ZTO-DV-500 and ZTO-DV-750 rate constants are determined to be 0.099 and 0.156 min−1, respectively, while at high concentration (10 mg L−1), these values are 0.043, and 0.091 min−1. Therefore, the ZTO-DV-750 composite has shown potent catalytic activity with NaBH4 over ZTO-DV-500 to decolourise organic dyes.

Stability, thermophysical properties, forced convective heat transfer, entropy minimization and exergy performance of a novel hybrid nanofluid: Experimental study

This research explores how incorporating graphene oxide (GO) into red mud (RM) creates a superior nanomaterial for heat transfer applications. RM's inherent stability and thermal conductivity (TC), stemming from its metal oxide composition, are further amplified by this hybrid nano-composite. The study primarily investigates the thermal performance of water-based RM mono nanofluid and hybrid RM + GO (50:50) nanofluids (HNFs) at nanoparticle concentrations of 0.1–0.75 vol%. An experimental setup consisting of a copper tube under turbulent flow conditions with a constant heat flux and a bulk fluid temperature of 60 °C was used to test the performance of HNF. Various techniques are used to characterize the nanoparticles (NPs), and evaluate the thermophysical properties of nanofluids. The experimental data reveal that the heat transfer coefficient (HTC) increases with higher inlet fluid velocity and nanoparticle concentrations. Notably, the HNF demonstrates a significant improvement of 47.2 % in Nusselt number (Nu) and a 13.6 % rise in pressure drop (Δp) compared to base fluid, at 0.75 vol%. The least entropy generation number (EGN) is obtained for the HNF (0.0049) compared to the RM NF (0.00583) at a concentration of 0.75 vol%. The exergy efficiency improves with an increase in concentration and Reynolds number (Re). Additionally, the study identifies the performance index (PI) of NFs and modelled correlations for estimating the Nu and friction factor (f) within the investigated concentration range.

Enhanced Oxygen Evolution Reaction Catalytic Properties of Novel Nanowire Structures from FeCo‐MOFs/GO via Low‐Temperature Annealing

Metal‐organic frameworks (MOFs) often suffer from poor stability, making them suitable precursors for metal oxides/porous carbon catalysts in the oxygen evolution reaction via pyrolysis. High‐temperature treatment, however, leads to significant loss of active sites. To address this, Fe‐MOFs, FeCo‐MOFs, and FeCo‐MOFs/graphene oxide (GO) composites using a one‐pot hydrothermal method are synthesized and annealed at a low temperature of 300 °C. Characterization reveals that FeCo‐MOFs/GO composites possess unique nanowire structures mixed with a small amount of nanoflakes. It is believed that introducing graphene oxide plays a critical role in forming this structure, because the defects in GO provide numerous nucleation sites for nanowire growth. With high specific surface area and good stability, these nanostructures show a low overpotential of 261.5 mV at a current density of 10 mA cm−2 and a Tafel slope of 20.47 mV dec−1 in 1 mol L−1 KOH alkaline water electrolysis. Density functional theory calculations further indicate that the synergistic effect of Fe and Co atoms enhances the catalytic activity.

Long-term addition of organic manure stimulates the growth and activity of comammox in a subtropical Inceptisol

The discovery of complete ammonia oxidizers (comammox) has dramatically altered our perception of nitrogen (N) biogeochemistry. However, their functional importance vs. the canonical ammonia oxidizers (i.e., ammonia oxidizing-archaea (AOA) and bacteria (AOB)) in agroecosystems is still poorly understood. Accordingly, a new assay using acetylene, 3,4-dimethylpyrazole phosphate (DMPP), and 1-octyne was adopted to assess the ammonia (NH3) oxidation and nitrous oxide (N2O) production activity of these functional guilds in a subtropical Inceptisol under long-term different fertilization regimes. These regimes include CK (no fertilizer control), synthetic fertilizer only (NPK), organic manure only (M) and organic manure plus synthetic fertilizer (MNPK). AOA dominated NH3 oxidation in the M treatment, while AOB dominated both NH3 oxidation and N2O production in all treatments except M. Comammox always played a minor role in both NH3 oxidation and N2O production across all treatments. Both M and MNPK treatments significantly increased the activity and growth of comammox. Compared to NPK, comammox exhibited increases of 270 % and 326 % in the NH3 oxidation rates, and increases of 1472 % and 563 % in the N2O production rates in M and MNPK, respectively. Random forest model revealed that copper (Cu), comammox abundance, and dissolved organic nitrogen (DON) were the most important predictors for the NH3 oxidation rates of comammox. Redundancy analyses (RDA) showed that fertilizer treatments significantly altered the community composition of NH3 oxidizers, and pH was the overarching parameter underpinning the community shift of the NH3 oxidizers. Overall, this study provides evidence that comammox play a minor yet unneglectable role in the nitrification of agroecosystems, and the long-term addition of organic manure stimulates the growth and activity of comammox in a subtropical Inceptisol.

Adsorption Study of Neodymium from the Aqueous Phase Using Fabricated Magnetic Chitosan-Functionalized Graphene Oxide Composites.

This work reports the performances of the magnetic chitosan@graphene oxide composite (MCh@GO) for the sorption of Nd(III) from aqueous medium. The prepared composite was synthesized by a coprecipitation method and then examined by FT-IR, XRD, SEM, and TGA. XRD analysis proved physical interactions between magnetic chitosan and graphene oxide through (inter- and intramolecular H-bonding and peptide bonding). TGA data approved the thermal stability of the prepared MCh@GO nanocomposite over their constituents. The optimum pH for the sorption process was 4.5. The Langmuir model and PSO fitted the experimental data. The adsorption process was found to be endothermic and spontaneous with a Q max of 56.6 mg g-1. Indeed, the MCh@GO composite proved to be an excellent adsorbent for the purification, remediation, and separation of Nd due to its promising properties.

Spectroscopic and statistical physics elucidation for Cu(II) remediation using magnetic bio adsorbent based on Fe3O4-chitosan-graphene oxide

Efficient harnessing of heavy metal pollution is an urgent environmental task. Herein, magnetic bio adsorbent (MB) based on Fe3O4-chitosan-graphene oxide composite was fabricated via one step co-precipitation for adsorptive remediation of Cu(II). Remediation efficiency was evaluated by batch adsorption, meanwhile adsorption mechanism was elucidated by spectroscopic tests (XPS, UV–Vis absorption and fluorescent emission spectra), statistical physics formalism, isotherm and kinetic fittings. Results show, MB reaches adsorption percent and quantity of 87.61 % and 350.43 mg·g−1 for Cu(II) in 30 min. By virtue of paramagnetism, MB can be readily recovered with a permanent magnet for easy regeneration and cyclic use, thereby retaining adsorption quantity 279.99 mg·g−1 at the fifth cycle. The Freundlich and pseudo second order model satisfactorily describes the adsorption, designating chemical interaction as the rate limiting step. Statistical physics calculation suggests two points. (1) Multi-ionic adsorption mechanism with exothermic, spontaneous and energy lowering feature. (2) Density of adsorption sites increases with temperature, resulting in improved adsorption capacity. Spectroscopic analysis confirms the involvement of CO, CO, -NH2 in Cu(II) uptake via electron donation. These explorations contribute with novel theoretical illumination for understanding both the thermodynamic feature and atomic scale mechanism of common pollutants adsorption by bio adsorbent like Fe3O4-chitosan-graphene oxide.

ZnO:CuO Composites Obtained by Rapid Joule Heating for Photocatalysis.

Semiconductor oxides belonging to various families are ideal candidates for application in photocatalytic processes. One of the challenges facing photocatalytic processes today is improving their efficiency under sunlight irradiation. In this study, the growth and characterization of semiconductor oxide nanostructures and composites based on the ZnO and CuO families are proposed. The selected growth method is the resistive heating of Zn and Cu wires to produce the corresponding oxides, combined with galvanic corrosion of Zn. An exhaustive characterization of the materials obtained has been carried out using techniques based on scanning electron microscopy and optical spectroscopies. The method we have followed and the conditions used in this study present promising results, not only from a degradation efficiency point of view but also because it is a cheap, easy, and fast growth method. These characteristics are essential in order to scale the process beyond the laboratory.

Microwave solvothermal synthesis and HTHP sintering of CoSb3/rGO composites: In-situ synthesis and enhanced thermoelectric properties

The utilization of CoSb3-based thermoelectric materials is currently confined to aviation applications, primarily attributed to their elevated thermal conductivity (κ) values. The incorporation of a nanostructuring approach, coupled with the introduction of a secondary phase, has demonstrated efficacy in diminishing the thermal conductivity (κ) values of CoSb3 materials. Here, the CoSb3/reduced graphene oxide (CoSb3/rGO) composites are obtained by sintering the as-synthesized powders, which ultra-fast synthesized in situ via microwave solvothermal method, under the High-temperature and High-Pressure (HTHP) conditions. The influence of reduced graphene oxide (rGO) on the structural and thermoelectric characteristics of CoSb3 composites has been systematically explored. In this study, CoSb3 nanoparticles with an average size of ∼33 nm exhibit uniform distribution, being effectively anchored onto the 2D sheets of rGO. In this work, the lattice thermal conductivity of CoSb3/rGO composites decreased with the addition of rGO. Based on the Debye-Callaway model, we attribute this to the effective scattering of phonons by the interface formed between the CoSb3 nanocrystals and the lamellar rGO. As a result, the CoSb3/rGO composite, containing 2 wt% graphene, exhibits a significantly enhanced maximum thermoelectric figure of merit (ZT) value, reaching ∼0.325 at 700 K. This represents an impressive improvement of approximately 300 % compared to the ZT value of the graphene-free CoSb3 bulk counterpart, which is ∼0.106. This study demonstrates the microwave solvothermal synthesis and HTHP sintering are in favor for an efficient, economical, and controllable synthesis of CoSb3/rGO composites, which provides a novel strategy for securing better thermoelectric performance.

Investigation of sodium–manganese oxides with various crystal phases for the efficient catalytic removal of diesel soot particles

Sodium–manganese oxides with various crystal phases (Na2Mn5O10, Na2Mn3O7, and Na4Mn9O18) were synthesized using a facile sol-gel method, and applied in the catalytic purification of soot particles from diesel engines. In this study, as-prepared samples with a single Na2Mn3O7 phase exhibited higher soot oxidation activity, with the lowest T10, T50, and T90 values of 279 ℃, 320 ℃, and 349 ℃, respectively. Numerous characterization techniques reveal that the Na2Mn3O7 catalysts have superior reducibility, NO oxidation, and storage capacity compared with the other crystal phases. In the meantime, the Na2Mn3O7 catalyst surface possesses a greater abundance of oxygen vacancies because of the emergence of Mn3+, which serve as crucial active sites during the dynamic cycling process of gaseous oxygen adsorption and activation. Moreover, the E-R reaction mechanism for soot combustion over the steps of (100) crystal plane of Na2Mn3O7 catalysts is proposed based on density functional theory (DFT) calculations and multiple characterization results. This study presents a facile and cost-efficient method for designing and preparing superior performance sodium–manganese composite oxides for soot combustion.

Study in the impact of quaternized graphene oxide (QGO) composition as modifier on the chemical, physical, mechanical, and performance properties of polyvinylidene fluoride (PVDF)-based nanocomposite membrane

Polyvinylidene Fluoride (PVDF) membranes were modified with quaternized graphene oxide (QGO) synthesized from graphene oxide and quaternized ammonium groups. PVDF/QGO membranes were created by blending PVDF and 0.01-0.05 g QGO via phase inversion. FTIR confirmed the successful QGO incorporation. PVDF/QGO membranes exhibited increased mechanical stiffness. Meanwhile, SEM revealed asymmetric morphology with surface and internal pores. AFM showed the membrane with 0.05 g and QGO had the highest surface roughness of 101.2 nm, which increased filtration area and flux. QGO improved hydrophilicity through hydroxyl and quaternary ammonium groups, enhancing water flux up to 1208 Lm?2h?1 for 0.05 g QGO. Cu2+ rejection increased to 75% for 0.05 g QGO membrane due to chelation and adsorption effects. PVDF/QGO membranes displayed bacterial growth inhibition, unlike pristine PVDF. The inhibition zone diameter increased with more QGO, indicating improved antibacterial activity. Overall, this study demonstrated that QGO improved PVDF membranes' hydrophilicity, antibacterial properties, and mechanical strength.

Solvent‐Free Efficient Hydrogenation of Levulinic Acid over Silicotungstic Acid Promoting the Activity of CuNiAl Catalysts: A Synergistic Effect

AbstractMulti‐metallic catalysts rely on the synergistic effect between metals to perform better catalytic effect in biomass hydrogenation experiments compared with mono‐metallic catalysts. A series of CuNiAl composite metal oxide catalysts promoted by silicotungstic acid (HSiW), which were prepared by co‐precipitation and impregnation methods, were characterized by powder X‐ray diffraction (XRD), N2‐physisorption, scanning electron microscope (SEM) and NH3 program temperature desorption (NH3‐TPD) and pyridine infrared adsorption (Py‐FTIR). Their catalytic performance was evaluated in the hydrogenation of levulinic acid (LA) to prepare γ‐valerolactone (GVL). The results showed that the addition of Cu could improve the hydrogenation activity of Ni, and the addition of HSiW could further increase the amount of acid sites in the catalysts. Both of them could enhance the conversion of LA to some extent. CuNiAl‐5SiW, the par excellence catalyst, relied on the synergistic interactions between metals as well as the Brønsted and Lewis acid active sites to show efficient hydrogenation performance. The CuNiAl‐5SiW catalyst demonstrated 96.9 % conversion of LA and more than 99 % selectivity to GVL under 2 hours of reaction time, 180 °C of reaction temperature, 3.0 MPa of initial hydrogen pressure and solvent‐free conditions.

Real-time coloration control of gallium-based strips through cold rolling.

Cold rolling has been used as a real-time surface oxidation control method to create colored strips on flexible substrates. By controlling the extrusion rate in real time, a variety of colored strips have been fabricated on Ga-based liquid metal (LM) strips. X-ray photoelectron spectroscopy (XPS) analysis shows that the surfaces of the colored strips, which were obtained through extrusion rate control of LM-Al, consist primarily of metal oxide composites, including Ga2O3, Ga2O, Al2O3, SnO2, and In2O3. The colors of the strip surfaces are directly correlated with the oxide film thickness. Additionally, these cold-rolled colored thin strips demonstrate high conductivity and have significant potential for use as conductive flexible components with indicator functions in the flexible electronics realm.

Unveiling Key Interface Characteristics of Ni/Yttria-Stabilized Zirconia Solid Oxide Cell Electrodes in H2O Electroreduction Using Operando X-ray Photoelectron Spectroscopy.

Nickel/yttria-stabilized zirconia (YSZ) composites are the most commonly used fuel electrodes for solid oxide cells. While microstructural changes of Ni/YSZ during operational conditions have been thoroughly investigated, there is limited knowledge regarding Ni/YSZ surface chemistry under working conditions. In this study, we examine the interaction between Ni/YSZ electrodes and water vapor under open circuit and polarization conditions, utilizing near ambient pressure soft and hard X-ray photoelectron spectroscopies. Miniature cells with conventional porous Ni/YSZ composite cermet cathodes were modified to facilitate the direct spectroscopic observation of the functional electrode's areas close to the interface with the YSZ electrolyte. The results highlight dynamic changes in the oxidation state and composition of Ni/YSZ under H2 and H2O atmospheres. We also quantify the accumulation of impurities on the electrode surface. Through adjustments in the pretreatment of the cell, the correlation between the nickel surface oxidation state and the cell's electrochemical performance during H2O electroreduction is established. It is unequivocally shown that nickel surface oxidation in H2O electrolysis favors NiO over Ni(OH)x, providing critical insights into the mechanism of Ni-phase redistribution within the electrode during long-term operation. Depth-dependent photoemission measurements, combined with theoretical quantitative simulations, reveal that NiO and Ni phases are uniformly mixed on the surface during H2O electrolysis. This differs from the conventional expectation of a NiO-shell/Ni-core configuration in gas phase oxidation. These findings provide crucial insights into the surface chemistry of Ni/YSZ electrodes under conditions relevant to H2O electrolysis, elucidating their impact on the electrochemical performance of the cell.