X-ray Absorption Near-edge Spectra Research Articles

Simultaneous removal of tetracycline hydrochloride and hexavalent chromium by heterogeneous Fenton in a photocatalytic fuel cell system

In this work, a novel double-chamber system (PFC-Fenton), combined photocatalytic fuel cell (PFC) with Fenton, was constructed for tetracycline hydrochloride (TCH) and hexavalent chromium (Cr(VI)) removal and electricity production. Therein, Zn5(OH)6(CO3)2/Fe2O3/BiVO4/fluorine-doped SnO2 (ZIO/BiVO4/FTO) and carboxylated carbon nanotubes/polypyrrole/graphite felt (CCNTs/Ppy/GF) were served as photoanode and cathode, respectively. Under light irradiation, the removal efficiencies of TCH and Cr(VI) with the addition of H2O2 (2 mL) could reach 93.1% and 80.4%, respectively. Moreover, the first-order kinetic constants (7.37 × 10−3 min−1 of TCH and 3.94 × 10−3 min−1 of Cr(VI)) were 5.26 and 5.57 times as much as the absence of H2O2. Simultaneously, the maximum power density could be obtained 0.022 mW/cm2 at a current density of 0.353 mA/cm2. Therein, the main contribution of TCH degradation was ·OH and holes in anode chamber. The synergistic effect of photoelectrons, generated ·O2−, and H2O2 played a crucial role in the reduction of Cr(VI) in cathode chamber. The high-performance liquid chromatography-mass spectrometry indicated that TCH could be partially mineralized into CO2 and H2O. X-ray photoelectron spectroscope and X-ray absorption near-edge structure spectra showed that Cr(VI) could be reduced to Cr(III). After 5 times of cycling, the removal efficiencies of TCH and Cr(VI) were still greater than 70%, indicating the remarkable stability of the PFC-Fenton system. Overall, this system could remove TCH/Cr(VI) and generate power simultaneously without iron sludge formation, demonstrating a promising method to further develop PFC-Fenton technology.

Construction of an Axial Charge Transfer Channel Between Single-Atom Fe Sites and Nitrogen-Doped Carbon Supports for Boosting Oxygen Reduction.

The introduction of axial-coordinated heteroatoms in Fe─N─C single-atom catalysts enables the significant enhancement of their oxygen reduction reaction (ORR) performance. However, the interaction relationship between the axial-coordinated heteroatoms and their carbon supports is still unclear. In this work, a gas phase surface treatment method is proposed to prepare a series of X─Fe─N─C (X = O, P, and S) single-atom catalysts with axial X-coordination on graphitic-N-rich carbon supports. Synchrotron-based X-ray absorption near-edge structure spectra and X-ray photoelectron spectroscopy indicate the formation of an axial charge transfer channel between the graphitic-N-rich carbon supports and single-atom Fe sites by axial O atoms in O─Fe─N─C. As a result, the O─Fe─N─C exhibits excellent ORR performance with a half-wave potential of 0.905V versus RHE and a high specific capacity of 884 mAh g-1 for zinc-air battery, which is superior to other X─Fe─N─C catalysts without axial charge transfer and the commercial Pt/C catalyst. This work not only demonstrates a general synthesis strategy for the preparation of single-atom catalysts with axial-coordinated heteroatoms, but also presents insights into the interaction between single-atom active sites and doped carbon supports.

Ultraviolet-B and Near-Infrared Dual-Band Luminescence in Bi3+/Bi2+ Codoped Persistent Phosphor for Optical Storage Application.

Discovering multifunctional luminescent materials to meet the demands of modern spectroscopy is of great significance. However, it is a standing challenge to enable multiple luminescence properties in a single material system via single metal ion doping. Here, we report the inherently Bi3+/Bi2+ codoped Ca3Ga2Ge3O12 persistent phosphor where Bi3+ is in situ reduced to Bi2+. This phosphor can act as an efficient multimodal luminescence material, which simultaneously exhibits long-lasting (>12 h) ultraviolet-B (UVB) and near-infrared (NIR) dual-band persistent luminescence after irradiation by 254 nm ultraviolet (UV) light. UVB and NIR afterglow are ascribed to the distinct Bi3+ and Bi2+ emitters, respectively, proven by comprehensive spectroscopic investigations including X-ray absorption near-edge structure spectra and X-ray photoelectron spectroscopy. Besides, this phosphor also exhibits exceptional photochromic features, accompanied by a rapid body color transformation from white to brown in response to 254 nm UV light within 60 s and excellent recovery capacity upon thermal or blue/white light stimulation. The combination of UVB persistent luminescence of Bi3+ and NIR afterglow of Bi2+ coupled with reversible white-to-brown photochromism phenomenon offers one type of promising multifunctional luminescence material, showing potential to be used for optical storage and anti-counterfeiting applications.

Boosting Multielectron Reaction Stability of Sodium Vanadium Phosphate by High-Entropy Substitution.

Na3V2(PO4)3 (NVP) based on the multielectron reactions between V2+ and V5+ has been considered a promising cathode for sodium-ion batteries (SIBs). However, it still suffers from unsatisfactory stability, caused by the poor reversibility of the V5+/V4+ redox couple and structure evolution. Herein, we propos a strategy that combines high-entropy substitution and electrolyte optimization to boost the reversible multielectron reactions of NVP. The high reversibility of the V5+/V4+ redox couple and crystalline structure evolution are disclosed by in situ X-ray absorption near-edge structure spectra and in situ X-ray diffraction. Meanwhile, the electrochemical reaction kinetics of high-entropy substitution NVP (HE-NVP) can be further improved in the diglyme-based electrolyte. These enable HE-NVP to deliver a superior electrochemical performance (capacity retention of 93.1% after 2000 cycles; a large reversible capacity of 120 mAh g-1 even at 5.0 A g-1). Besides, the long cycle life and high power density of the HE-NVP∥natural graphite full-cell configuration demonstrated the superiority of HE-NVP cathode in SIBs. This work highlights that the synergism of high-entropy substitution and electrolyte optimization is a powerful strategy to enhance the sodium-storage performance of polyanionic cathodes for SIBs.

Generalization of One-Center Nonorthogonal Configuration Interaction Singles to Open-Shell Singlet Reference States: Theory and Application to Valence-Core Pump-Probe States in Acetylacetone.

We formulate a one-center nonorthogonal configuration interaction singles (1C-NOCIS) theory for the computation of core excited states of an initial singlet state with two unpaired electrons. This model, which we refer to as 1C-NOCIS two-electron open-shell (2eOS), is appropriate for computing the K-edge near-edge X-ray absorption spectra (NEXAS) of the valence excited states of closed-shell molecules relevant to pump-probe time-resolved (TR) NEXAS experiments. With the inclusion of core-hole relaxation effects and explicit spin adaptation, 1C-NOCIS 2eOS requires mild shifts to match experiment, is free of artifacts due to spin contamination, and can capture the high-energy region of the spectrum beyond the transitions into the singly occupied molecular orbitals (SOMOs). Calculations on water and thymine illustrate the different key features of excited-state NEXAS, namely, the core-to-SOMO transitions as well as shifts and spin-splittings in the transitions analogous to those of the ground state. Simulations of the TR-NEXAS of acetylacetone after excitation to its π → π* singlet excited state at the carbon K-edge, an experiment carried out recently, showcase the ability of 1C-NOCIS 2eOS to efficiently simulate NEXAS based on nonadiabatic molecular dynamics simulations.

OER activate NixCo(1-x) NPs to NixCo(1-x)(OH)2 on cobalt foam with excellent supercapacitors performance

5-6 nm hydrophilic NixCo(1-x) NPs was synthesized by a cost-effective and scalable method and was coated onto conductive substrates without any binders or additives thanks to its small particle effect and possiblely magnetic effects. Then, the NixCo(1-x) NPs can be transformed into NixCo(1-x)(OH)2 by an OER-activating strategy. Optimized by the composition effect, the Ni0.8Co0.2/CF exhibits best activity for supercapacitors (2124F/g). Underling mechanism of the OER evolution process well studied by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectrometry, X-ray absorption near-edge spectra (XANES). Density functional theory (DFT) calculations was performed and verify the synergistic effect of nickel and cobalt and the support effect.

Direct extraction of structural insight from X-ray absorption near-edge spectra using convolutional neural networks

Direct extraction of structural insight from X-ray absorption near-edge spectra using convolutional neural networks

Dynamics of femtosecond heated warm dense copper with time-resolved L3-edge XANES.

Combining experimental set up and ab initio molecular dynamics simulations, we were able to follow the time evolution of the X-ray absorption near edge spectrum (XANES) of a dense copper plasma. This provides a deep insight into femtosecond laser interaction with a metallic copper target. This paper presents a review of the experimental developments we made to reduce the X-ray probe duration, from approximately 10 ps to fs duration with table-top laser systems. Moreover, we present microscopic scale simulations, performed with Density Functional Theory, as well as macroscopic simulations considering the Two-Temperature Model. These tools allow us to get a complete picture of the evolution of the target at a microscopic level, from the heating process to the melting and expansion stages, with a clear view of the physics involved during these processes. This article is part of the theme issue 'Dynamic and transient processes in warm dense matter'.

Toward Tungsten Electrodeposition at Moderate Temperatures Below 100 °C Using Chloroaluminate Ionic Liquids

The electrodeposition of tungsten at moderate temperatures (<100 °C) has been of significant interest for the fabrication of thin films and microelectromechanical system components to decrease energy consumption and increase process safety. In this study, we investigated the electrochemical reduction of WCl4 and WCl5 in 1-ethyl-3-methylimidazolium chloride (EMIC) and EMIC–AlCl3 ionic liquids at 80 °C–120 °C. W-rich films with a thickness of approximately 1 μm were obtained from the Lewis acidic EMIC–AlCl3–WCl5 bath, whereas the other baths did not yield any deposits. The films obtained from the EMIC–AlCl3–WCl5 bath at 80 °C had higher W contents of 54 at.% than those obtained at 120 °C. X-ray absorption near-edge structure spectra of the W-rich films indicated that W existed in an oxidized state. The findings of this study can be used as a guide to explore optimal electrolytes and electrolytic conditions for the electrodeposition of metallic W at moderate temperatures.

Selenium/sulfur-modified montmorillonite materials mitigate mercury pollution in farmland

Selenium (Se) amendment could reduce mercury (Hg) bioaccumulation in crops, but sometimes it could cause excessive Se accumulation in crops and potential Se exposure risks for humans. In this study, we designed and synthesized selenium and sulfur-modified montmorillonite materials (Se/S-Mont) to effectively reduce mercury levels and avoid excessive Se enrichment in plants. The results of pot experiments (1 g Se/S-Mont/100 g soil) and field microplot trials (0.3 g Se/S-Mont/100 g soil, 8 t/ha) showed that Se/S-Mont amendments significantly reduced the Hg concentrations in water spinach and hybrid Pennisetum by 28–68% and 57%–92% (P < 0.05), respectively, while they did not lead to excessive Se bioaccumulation in the plants. Se/S-Mont was more efficient in mitigating soil Hg pollution than adding raw materials (e.g., NaSeO₃) and their combinations, and they significantly reduced the available Se fraction in the soil and the Se levels in the plants (P < 0.05). The potential mechanisms revealed by X-ray absorption near-edge spectra (XANES) and pot experiments were the adsorption and slow release of Hg, S, and Se by Se/S-Mont, the high affinity between Hg and Se, competition between Se and S, and the formation of stable complexes containing Se–S–Hg. The Se/S-Mont immobilizer was easy to prepare and required the application of small amounts, and the remediation effect was relatively stable and exhibited few negative effects; therefore, the approach showed high environmental and economic potentials.

Mild nitridation of perovskite manganite: Synthesis, structure and magnetism

The nitrogen lightly doped perovskite manganite La0.5Ba0.5MnO(3-δ)-xNx was synthesized following a mild nitridation strategy by optimizing annealing temperature, annealing time and NH3/Ar flow rate ratio. Neutron powder diffraction (NPD) characterization evidences an N-doping triggered structural phase transition from pseudo-cubic Pm-3m to tetragonal P4/mmm and further confirms a preferable substitution at O1 and O2 sites closing to the Ba-rich layers. N 1s K-edge X-ray absorption near edge spectrum (XANES) with total fluorescence yield (TFY) mode, X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FT-IR) spectroscopy collectively convince the Mn–N bonded state. The O/N atomic ratio is determined to be 2.26/0.22 by XPS analysis closing to the value of 2.25/0.18 from NPD refinement. Magnetic property characterization reveals that both long-range Mn3+-O-Mn4+ ferromagnetic coupling and high Curie temperature (TC) are maintained upon N-doping. Besides, significant spin frozen with robust domain pinning is identified below TC which can be ascribed to the short-range Mn–N–Mn clusters and/or oxygen defects. This work expands the connotation of transition-metal based perovskite oxynitride and may inspire the development of photosensitive semiconductor device with magnetic response.

Pseudocapacitive Deionization of Saltwater by Mn3O4@C/Activated Carbon.

Capacitive deionization (CDI), a m ethod with notable advantages of relatively low energy consumption and environmental friendliness, has been widely used in desalination of saltwater. However, due to the weak electrical double-layer electrosorption of ions from water, CDI has suffered from low throughput capacity that may limit its commercial applications. Thus, it is of importance to develop a high-efficiency and engineering-feasible CDI process. Manganese and cobalt and their oxides, being faradic materials, have a relatively high pseudocapacitance, which can cause an increase of positive and negative charges on opposing electrodes. However, their low conductivity properties limit their electrochemical applications. Pseudocapacitive Mn3O4 nanoparticles encapsulated within a conducting carbon shell (Mn3O4@C) were prepared to enhance charge transfer and capacitance for CDI. Desalination performances of the Mn3O4@C (5-15 wt %) core-shell nanoparticles on activated carbon (AC) (Mn3O4@C/AC) serving as CDI electrodes have thus been investigated. The pseudocapacitive Mn3O4@C/AC electrodes with relatively low diffusion resistances have much greater capacitance (240-1300 F/g) than the pristine AC electrode (120 F/g). In situ synchrotron X-ray absorption near-edge structure spectra of the Mn3O4@C/AC electrodes during CDI (under 1.2 and -1.2 V for electrosorption and regeneration, respectively) demonstrate that reversible faradic redox reactions cause more negative charges on the negative electrode and more positive charges on the positive electrode. Consequently, the pseudocapacitive electrodes for CDI of saltwater ([NaCl] = 1000 ppm) show much better desalination performances with a high optimized salt removal (600 mg/g·day), electrosorption efficiency (48%), and electrosorption capacity (EC) (25 mg/g) than the AC electrodes (288 mg/g·day, 23%, and 12 mg/g, respectively). The Mn3O4@C/AC electrode has a maximum EC of 29 mg/g for CDI under +1.2 V. Also, the Mn3O4@C/AC electrodes have much higher pseudocapacitive electrosorption rate constants (0.0049-0.0087 h-1) than the AC electrode (0.0016 h-1). This work demonstrates the feasibility of high-efficiency CDI of saltwater for water recycling and reuse using the low-cost and easily fabricated pseudocapacitive Mn3O4@C/AC electrodes.

Deciphering the Structural and Chemical Transformations of Oxide Catalysts during Oxygen Evolution Reaction Using Quick X-ray Absorption Spectroscopy and Machine Learning.

Bimetallic transition-metal oxides, such as spinel-like CoxFe3-xO4 materials, are known as attractive catalysts for the oxygen evolution reaction (OER) in alkaline electrolytes. Nonetheless, unveiling the real active species and active states in these catalysts remains a challenge. The coexistence of metal ions in different chemical states and in different chemical environments, including disordered X-ray amorphous phases that all evolve under reaction conditions, hinders the application of common operando techniques. Here, we address this issue by relying on operando quick X-ray absorption fine structure spectroscopy, coupled with unsupervised and supervised machine learning methods. We use principal component analysis to understand the subtle changes in the X-ray absorption near-edge structure spectra and develop an artificial neural network to decipher the extended X-ray absorption fine structure spectra. This allows us to separately track the evolution of tetrahedrally and octahedrally coordinated species and to disentangle the chemical changes and several phase transitions taking place in CoxFe3-xO4 catalysts and on their active surface, related to the conversion of disordered oxides into spinel-like structures, transformation of spinels into active oxyhydroxides, and changes in the degree of spinel inversion in the course of the activation treatment and under OER conditions. By correlating the revealed structural changes with the distinct catalytic activity for a series of CoxFe3-xO4 samples, we elucidate the active species and OER mechanism.

Probing the Local Environment of Al-Substitution into Ferrihydrite Using DFT + U Calculations

Ferrihydrite (Fh) is a poorly crystalline oxyhydroxide that has attracted attention due to its importance in geochemistry, ion mobility, adsorption, and as a precursor for the formation of more crystalline phases such as goethite and hematite. A chemical model for the isomorphic substitution of the Fe sites by Al is proposed. DFT/plane wave calculations have been performed to provide information about the local environment of Al-substitution into Fh. The structural and electronic properties have been investigated in detail. Al prefers to replace the octahedral Fe sites, which has been evidenced by the comparison of the calculated Al K-edge X-ray absorption near-edge structure spectra with the available experimental data. The effect of the increasing ionicity of the system upon Al-substitution to the quadrupolar coupling constant of 27Al NMR and the Mössbauer quadrupole splitting and isomer shift parameters have been investigated. The results indicate that these parameters are affected by the concentration of Fe-substituted sites. Al-substitution increases the band gap dispersion with the formation of Al electronic states in the conduction band. The standard Helmholtz free energy of Al-substitution has been estimated and discussed in detail.

Uncertainty quantification of spectral predictions using deep neural networks.

We investigate the performance of uncertainty quantification methods, namely deep ensembles and bootstrap resampling, for deep neural network (DNN) predictions of transition metal K-edge X-ray absorption near-edge structure (XANES) spectra. Bootstrap resampling combined with our multi-layer perceptron (MLP) model provides an accurate assessment of uncertainty with >90% of all predicted spectral intensities falling within ±3σ of the true values for held-out data across the nine first-row transition metal K-edge XANES spectra.

Operando X-ray Absorption Spectroscopy Study of SnO2 Nanoparticles for Electrochemical Reduction of CO2 to Formate

Tin-based electrocatalysts exhibit a remarkable ability to catalyze CO2 to formate selectively. Understanding the size-property relationships and exploring the evolution of the active size still lack complete understanding. Herein, we prepared SnO2 nanoparticles (NPs) with a controllable size supported on commercial carbon spheres (SnO2/C-n, n = 1, 2, and 3) by a simple low-temperature annealing method. The transmission electron microscopy/scanning transmission electron microscopy images and fitting results of the small-angle X-ray scattering profile confirm the increased size of SnO2 NPs due to the increase of SnO2 loading. The catalytic performance of SnO2 has proved the size-dependent effect during the CO2 reduction reaction process. The as-prepared SnO2/C-1 displayed the maximum Faradic efficiency of formate (FEHCOO-) of 82.7% at -1.0 V versus reversible hydrogen electrode (RHE). In contrast, SnO2/C-2 and SnO2/C-3 with larger particle sizes achieved lower maximum FEHCOO- and larger overpotential. Moreover, we employed operando X-ray absorption spectroscopy to study the evolution of the oxidation state and local coordination environment of SnO2 under working conditions. In addition to the observed shifts of the rising edge of Sn K-edge X-ray absorption near-edge structure spectra to a lower energy side as the applied voltage decreases, the decreased coordination number of Sn in the Sn-O scattering path and the presence of Sn metal contribution in the extended X-ray absorption fine structure spectra verify the reduction of SnO2 to SnOx and metallic Sn.

Investigation of lattice dynamics, magnetism, and electronic transport in β−Na0.33V2O5

We investigate the electronic and magnetic properties as well as lattice dynamics and spin-phonon coupling of $\beta$-Na$_{0.33}$V$_2$O$_5$ using temperature-dependent Raman scattering, dc-magnetization and dc-resistivity, x-ray photoemission, and absorption spectroscopy. The Rietveld refinement of XRD pattern with space group C2/m confirms the monoclinic structure. The analysis of temperature-dependent Raman spectra in a temperature range of 13--673~K reveals an anharmonic dependence of the phonon frequency and full width at half maximum, which is accredited to the symmetric phonon decay. However, below about 40 K, the hardening of the phonon frequency beyond anharmonicity is attributed to the spin-phonon coupling. Interestingly, the estimated effective magnetic moment $\mu_{\rm eff}=$ 0.63~$\mu_B$ from the magnetization data manifests a mixed-valence state of V ions in 4+ (18$\pm$1\%) and 5+ (82$\pm$1\%). A similar ratio of V$^{4+}$ to V$^{5+}$ is also observed in the x-ray photoemission and x-ray absorption near-edge spectra and that is found to be consistent with the sample stoichiometry. In addition, the V$^{4+}$ ions are distributed between different vanadium (V1 and V3) sites. The analysis of extended x-ray absorption fine structure at different V-sites gives the corresponding V--O bond lengths, which are utilized in the assignment of Raman modes. Moreover, the temperature-dependent resistivity resembles a semiconducting behavior where the charge carrier transport is facilitated by the band conduction at higher temperatures and via hopping $\le$260~K.

Effect of Ginkgo biloba leaves on the removal efficiency of Cr(VI) in soil and its underlying mechanism

Cr(VI) is a toxic, teratogenic, and carcinogenic heavy metal element in soil that poses major ecological and human health risks. In this study, microcosm tests combined with X-ray absorption near-edge spectra (XANES) and 16Sr DNA amplification techniques were used to explore the effect of Ginkgo biloba leaves on the removal efficiency of Cr(VI) in soil and its underlying mechanism. Ginkgo biloba leaves had a favorable remediation effect on soil varying in Cr(VI) contamination levels, and the optimal effect was observed when 5% Ginkgo biloba leaves were added. The occurrence state of Cr(VI) in soil before and after the addition of Ginkgo biloba leaves was analyzed by XANES, which revealed that Cr(VI) was fully converted to the more biologically innocuous Cr(III), and the hydroxyl-containing quercetin in Ginkgo biloba leaves was one of the primary components mediating this reduction reaction. The Cr(VI) content was significantly lower in non-sterilized soil than in sterilized soil, suggesting that soil microorganisms play a key role in the remediation process. The addition of Ginkgo biloba leaves decreased the α-diversity and altered the β-diversity of the soil bacterial community. Actinobacteria was the dominant phylum in the soil remediated by Ginkgo biloba leaves; four genera of Cr(VI)-reducing bacteria were also enriched, including Agrococcus, Klebsiella, Streptomyces, and Microbacterium. Functional gene abundances predicted by PICRUST indicated that the expression of glutathione synthesis genes was substantially up-regulated, which might be the main metabolic pathway underlying the mitigation of Cr(VI) toxicity in soil by Cr(VI)-reducing bacteria. In sum, Ginkgo biloba leaves can effectively remove soil Cr(VI) and reduce Cr(VI) to Cr(III) via quercetin in soil, which also functions as a carbon source to drive the production of glutathione via Cr(VI)-reducing bacteria and mitigate Cr(VI) toxicity. The findings of this study elucidate the chemical and microbial mechanisms of Cr(VI) removal in soil by Ginkgo biloba leaves and provide insights that could be used to enhance the remediation of Cr(VI)-contaminated soil.

Multiple Coordination of Chromium Ion Luminescence: A Strategy for Designing Ultra-broadband NIR Long Persistent Luminescent Materials.

Near-infrared (NIR) long persistent luminescent (LPL) materials have attracted the interest of many researchers as they have potential applications in many aspects. However, majority of studies on Cr3+ ion-doped LPL materials have focused on Cr3+ in an octahedral site, and the luminescence is limited to the short-wavelength NIR-I region (700-900 nm), which is detrimental to fully explore Cr3+ ion-doped LPL materials with potential applications. In this work, a novel ultra-broadband NIR LPL material, Na2CaGe6O14 (NCGO):x%Cr3+, was successfully designed and synthesized, covering the luminescence range of 600-1200 nm and having the best afterglow duration of more than 10 h. Combining the luminescence lifetime with the low-temperature spectrum, it was concluded that the luminescence of NCGO:Cr3+ consists of the co-emission of Cr3+ in octahedra and tetrahedra. And it was confirmed by electron paramagnetic resonance (EPR) spectrum and X-ray absorption near-edge spectrum (XANES). The application prospects of NCGO:x%Cr3+ in many aspects were investigated in detail. This work could not only give a reference for researchers to study Cr3+ luminescence in multiple coordination but also provide a new strategy for obtaining new ultra-broadband NIR LPL materials.

Heating up the OER: Investigation of IrO2 OER Catalysts as Function of Potential and Temperature**

AbstractDespite intensive investigations for unravelling the water splitting reaction, the catalyst behavior during the oxygen evolution reaction (OER) is still not fully understood. This is especially true under more demanding conditions like high potentials and high temperatures. Rotating disk electrode measurements show a gradual increase of OER current when increasing the temperature up to 80 °C. However, strong bubble formation at elevated temperatures makes in‐situ characterization of the catalyst challenging. Here we utilize an in‐situ electrochemical and heated flow cell, which aims at an efficient removal of bubbles from the catalyst surface and enables structural studies by X‐ray absorption spectroscopy (XAS) at temperatures up to 80 °C. Changes in the Ir L3‐edge X‐ray absorption near edge spectra (XANES) were observed with respect to the white line position and principal components related to structural changes were extracted. At temperatures of 60 °C and above, the white line position of XANES spectra reaches a steady state, which is possibly caused by an equilibrium of different Ir oxidation states. These findings provide first spectroscopic insights in the behavior of OER catalysts at elevated temperatures which are typical for industrial applications and rarely addressed until now.