X-ray Photoelectron Spectroscopy Data Research Articles

NH3-probe X-ray photoelectron spectroscopy method to characterize solid acidity of clay minerals

Accurate determination of solid acidity is essential for evaluating the catalytic activity of clay minerals. However, the conventional Fourier-transform infrared (FTIR) method using NH3 as the probe encounters challenges in measuring the solid acidity owing to the presence of water on the surface or within interlayer spaces of clay minerals as well as the influence of environmental water during the detection process. To mitigate water interference, a NH3-probe X-ray photoelectron spectroscopy (XPS) approach was adopted as an alternative to the FTIR method for the identification and semi-quantification of solid acidity of clay minerals. Following NH3 adsorption, the types of solid acid sites in clay minerals were identified through the chemical shift in N1s XPS spectra. The ratio of Brønsted and Lewis acid sites in a given sample and the relative concentration of acid sites across different samples were determined by examining the specific N1s peak area ratio. According to the XPS data, the ratios of Brønsted and Lewis acid sites in Ca-montmorillonite (SAz-2) and Na-montmorillonite (SWy-2) were nearly 1:1, whereas that for the illite–smectite mixed-layer mineral (ISCz-1) was 4. The acid site contents in SAz-2 were more than twice those of SWy-2. This work highlights the promising application prospects of the NH3-probe XPS method in solid acidity investigations of clay minerals.

Effects of porous structure and oxygen functionalities on electrochemical synthesis of hydrogen peroxide on ordered mesoporous carbon

Two-electron oxygen reduction reaction (2e− ORR) is a promising alternative to energy-intensive anthraquinone process for hydrogen peroxide (H2O2) production. Metal-free nanocarbon materials have garnered intensive attention as highly prospective electrocatalysts for H2O2 production, and an in-depth understanding of their porous structure and active sites have become a critical scientific challenge. The present research investigates a range of porous carbon catalysts, including non-porous, microporous, and mesoporous structures, to elucidate the impacts of porous structures on 2e− ORR activity. The results highlighted the superiority of mesoporous carbon over other porous materials, demonstrating remarkable H2O2 selectivity. Furthermore, integration of X-ray photoelectron spectroscopy (XPS) data analysis with electrochemical assessment results unravels the moderate surface oxygen content is the key to increase 2e− ORR activity. These results not only highlight the intricate interplay between pore structure and oxygen content in determining catalytic selectivity, but also enable the design of carbon catalysts for specific electrochemical reactions.

Influence of cationic vacancy diffusion on the aging behavior of low-temperature SrCo1-xRuxO3 thermosensitive ceramics

The thermosensitive ceramics of negative temperature coefficient (NTC), SrCo1-xRuxO3 (0 ≤ x ≤ 0.8), were synthesized using the solid-phase method. The research systematically explored the phase structure, microstructure, elemental chemical states, electrical properties, and aging performance. X-ray diffraction (XRD) data indicates that with the increase of Ru content, the lattice parameter increases. Scanning electron microscopy (SEM) images reveal a dense and uniform microstructure. X-ray photoelectron spectroscopy (XPS) data indicates the presence of Co2+/Co3+ and Ru4+/Ru5+ ion pairs. Resistive temperature data indicates its potential use as a low-temperature thermosensitive resistance material in the range of 2–300 K. Fitting the resistance-temperature curve using the thermally activated band conduction model and Mott's 3D variable range hopping model. Proposed the Ru–O2--Co hopping model, elucidating the hole hopping transport mechanism in NTC ceramics. Impedance spectroscopy analysis indicates that grain boundary resistance dominates the overall resistance of the sample. After aging at 77 K for 864 h, the maximum aging drift rate of the ceramic material is 1.55 %. Proposed a novel cationic vacancy diffusion model to explain aging phenomena, offering a new perspective for designing high-stability low-temperature NTC thermistors.

Characteristics of the incorporation of Yb defect states in CuO:ZnO nanocomposite

Exploring magnetic order in nonferromagnetic substances, such as CuO:ZnO, becomes especially attractive when introducing defect states through nonmagnetic ion doping. In this study, we delved into the impact of Yb doping on the structural, morphological, optical, and magnetic properties of CuO:ZnO. The Yb doped CuO:ZnO was prepared with different Yb concentrations (x = 0.00–20 %) via the temperature-assisted co-precipitation method. X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), field emission scanning electron microscopy (FE-SEM), high resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared spectroscopy (FTIR), UV–Vis spectroscopy, and vibrating sample magnetometer (VSM) were used to investigate the structural, morphological, optical, and magnetic properties of Yb doped CuO:ZnO nanocomposites.The incorporation of Yb in CuO:ZnO nanocomposites leads to a notable shift of the characteristic XRD peaks of CuO and ZnO to lower angles, accompanied by an increase in the lattice parameters. UV–visible absorption spectroscopy shows an overall decrease in the optical band gap energy of ZnO as the Yb defect level increases. FE-SEM studies revealed the transformation of spherical structures into agglomerated non-spherical structures upon the introduction of Yb ions into CuO:ZnO nanocomposites. According to XPS data, the predominant valences of Yb-doped CuO:ZnO nanocomposites are Zn2+, Cu2+, and Yb3+. One noteworthy observation from the XPS results is that, in comparison to the intensity of OL or Oad peaks, the intensity of OV (Oxygen vacancy) defect peak increases when the Yb impurity concentration increases. Magnetic measurements demonstrated a diamagnetic order in pure ZnO, which converts to a ferromagnetic order with the incorporation of Yb defect states. The ferromagnetic properties of the Yb-doped CuO:ZnO nanocomposite can be ascribed to the exchange interaction of Yb3+ ions with defect states (Oxygen Vacancy) in ZnO and CuO.

Degradation of Methyl Red (MR) dye via fabricated Y2O3–MgO/g-C3N4 nanostructures: Modification of band gap and photocatalysis under visible light

In this study, graphitic carbon nitride (g-C3N4) composites with metal oxide nanoparticles (Y2O3, MgO) and their combination (CN, YCN, MCN and YMCN) were synthesized by an ultrasonic technique and were then characterized by different tools such as UV–Vis diffuse reflectance spectroscopy (DRS), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) analysis and X-ray photoelectron spectroscopy (XPS). From the XRD diffractograms of the YMCN ternary composite, the g-C3N4, cubic MgO and Y2O3 structural phases were identified. The morphology of the as prepared nanostructure from the SEM analysis revealed the dispersion of the metal oxides nanoparticles with the graphitic sheets and the presence of the corresponding elements were confirmed by the EDX and XPS data. The FT–IR bands confirmed the bonding of the metal oxides to the nitride host as indicated by the characteristic modes. A reduction of the band gap energies was confirmed by the UV–Vis to indicate its visible light possible photoactivity. Accordingly, its visible light driven photocatalytic performance was assessed for methyl red degradation. The degradation competence was highest for the ternary composite YMCN due to the coupling of the semiconductors which increases the absorption and the charge carriers’ separation as well. The kinetics of degradation was best described by pseudo-first-order, and the most active species were the holes and the hydroxyl radicals. Thus, the YMCN nanocomposite is a visible light-active photocatalyst which can be engaged in the degradation of organic pollutants.

Role of Nd doping on the structural, morphological and optical properties of BaTiO3 nanoparticles hydrothermally synthesized

Herein, we have reported the facile synthesis of pure and neodymium (Nd)-doped BaTiO3 powders via the hydrothermal method. The effects of Nd concentration (2–10 wt %) on the properties of the BaTiO3 powders were studied. Structural and morphological characteristics were realized using X-ray diffraction (XRD), scanning electronic microscopy (SEM), energy dispersive X-ray (EDS), and X-ray photoelectron spectroscopy (XPS). Fourier transform infrared (FT-IR), UV–visible, and photoluminescence (PL) spectroscopies were used for optical analyses. XRD results show that all powders crystallized under a cubic structure with an average crystallite size that was in the range of 35–47 nm. SEM micrographs revealed that the grains were spherical-shaped, with an average size found in the range of 232–390 nm. The EDS analysis detected the presence of Ba, Ti, O, and Nd elements in the elaborate materials. XPS data confirms the introduction of Nd3+ in the BaTiO3 and the amphoteric substitution of Nd3+ in the Ba and Ti sites at 6 and 10 wt%. FT-IR spectra indicate the presence of the Ti–O vibration bonds. UV–visible optical spectra illustrate the enhancement of absorbance with Nd doping. PL spectra exhibit ultraviolet, blue, green, and orange emissions in the samples.

AC-Modulated XPS Enables to Externally Control the Electrical Field Distributions on Metal Electrode/Ionic Liquid Devices.

X-Ray Photoelectron Spectroscopy (XPS) has been utilized to extract local electrical potential profiles by recording core-level binding energy shifts upon application of the AC [square-wave (SQW)] bias with different frequencies. An electrochemical system consisting of a coplanar capacitor with a polyethylene membrane (PEM) coated with the Ionic Liquid (IL) N,N-diethyl-N-methyl-N-(2-methoxyethyl) ammonium bis(trifluoromethanesulfonyl)imide (DEME-TFSI) as the electrolyte is investigated. Analyses are carried out in operando, such that XPS measurements are recorded simultaneously with current measurements. ILs have complex charging/discharging processes, in addition to the formation of Electrical Double Layers (EDL) at the interfaces, and certain properties of these processes can be captured using AC modulation within appropriate time windows of observation. Herein, we select two frequencies, namely, 10 kHz and 0.1 Hz, to separate effects of the fast polarization and slow migratory motions, respectively. Moreover, the local potential developments after adding two equivalent series resistors at three different physical positions of the device have been carefully evaluated from the binding energy shifts in the F 1s peak representing the anion of the IL. This circuit modification allows us to quantify the AC currents passing through the device, as well as the system's impedance, in addition to revealing the potential variations due the IR drops. The complex AC-modulated local XPS data recorded can also be faithfully reproduced using the unmodulated F 1s spectrum and by convoluting it with electrical circuit output provided by the LT-Spice software. The outcome of these efforts is a more realistic equivalent circuit model, which can be related to chemical/physical makeup of the electrochemical system. An important finding of this methodology emerges as the possibility to induce additional local electrical field developments within the device, the directions of which can be reversed controllably.

Surface science insight note: Charge compensation and charge correction in X‐ray photoelectron spectroscopy

Strategies to deal with sample charging effects on X‐ray photoelectron spectroscopy (XPS) spectra are presented. These strategies combine charge compensation (or lack of) via a flow of electrons and an electrical connection (or lack of) of samples to the ground. Practical examples involving samples with a range of different electrical properties, sample structure/composition and sensitivity to X‐rays, illustrate the correlation between sample properties, measurement strategies, and the resulting XPS data. The most appropriate measurement strategy for a particular sample is also recommended. We highlight the crucial importance of appropriate XPS data acquisition to obtain a correct data interpretation.

Biosynthesis and characterization of selenium nanoparticles by Se-tolerant Lactiplantibacillus plantarum

Selenium nanoparticles synthesized by Lactobacillus (LacSeNPs) are considered the safer form of selenium supplementation. This study synthesized a new LacSeNPs by a selenium-tolerant strain Lactiplanibacillus plantarum BSe, and investigate its characteristics, antibacterial activity, and cytotoxicity. The results showed that L. plantarum BSe could grow at Se(Ⅳ) concentrations of 100 mmol L−1, and achieving a conversion level of 76.32% of selenium into LacSeNPs. Electron microscopy, FT-IR and X-ray photoelectron spectroscopic data indicated that only elemental Se existed in LacSeNPs and was encapsulated by proteins and polysaccharides, and the atomic proportion was Se (24.83%), accompanied with C (67.03%), N (3.12%), O (4.24%) and S (0.78%). LacSeNPs showed strong inhibition to Escherichia coli and Staphylococcus aureus. Furthermore, at equivalent selenium concentrations, LacSeNPs exhibits lower cytotoxicity compared to selenite. The findings of this study demonstrate that Lactiplanibacillus plantarum BSe is an excellent LacSeNPs synthesis bacterium and has potential application value in the production of SeNPs food additives.

Synthesis and Study of Superhigh-Concentrated Organosols of Silver Nanoparticles

Abstract Due to their unique properties, organosols of silver nanoparticles are widely used in optical and semiconductor devices, to produce electrically and thermally conductive films, as catalysts, antibacterial materials, etc. This work proposes a simple and highly productive method for the preparation of silver organosols, which have a metal concentration as high as 1800 g/L and contain spherical nanoparticles with low polydispersity and a median size of 9.1 nm. The method consists in the initial preparation of silver nanoparticle hydrosols with a concentration of higher than 30 g/L followed by the transfer of the NPs into an organic phase of o-xylene. A set of physical research methods has been employed to study the regularities of the extraction of silver nanoparticles with o-xylene in the presence of cetyltrimethylammonium bromide (CTAB) and ethanol and to determine the optimal process conditions, under which the extraction degree is as high as 62.5%. It has been found that bromine anions contained in CTAB molecules cause the aggregation of some amount of silver nanoparticles with the formation of silver metal sediment in the aqueous phase. According to X-ray photoelectron spectroscopy data, the sediment contains bromide ions (up to 4 at %) on the particle surface. Organosols synthesized under optimal conditions are stable for more than 7 months and withstand repeated cycles of drying and redispersing. Silver organosols have been used to obtain metal films with an electrical conductivity of about 68 500 S/cm, which increases to 412 000 and 509 500 S/cm (87.8% of the electrical conductivity of bulk silver) after thermal treatment at 150 and 250°C, respectively.

NEXAFS and XPS Studies of Co Doped Bismuth Magnesium Tantalate Pyrochlores

Co doped bismuth magnesium tantalate with a pyrochlore structure (sp. gr. Fd-3m) was synthesized for the first time using the standard ceramic method. Single phase Bi2Mg1−xCoxTa2O9 samples were found to be formed when x < 0.7 in the X-ray phase analysis. However, with a higher cobalt content in the samples, the impurity phase β-BiTaO4 (sp. gr. P-1) is detected, and its amount is proportional to the degree of cobalt doping. The formation of solid solutions is evidenced by a uniform increase in the unit cell parameter of the Co,Mg co doped bismuth tantalate phase with an increase in the content of cobalt ions in the samples from 10.5412(8) (x = 0.3) to 10.5499(8) Å (x = 0.7). The samples exhibit a porous microstructure consisting of chaotically oriented and partially fused elongated grains measuring 1–2 μm. The dependence of the ceramic grain size on the n(Mg)/n(Co) ratio was not determined. X-ray spectroscopy (ear dge X-ray bsorption ine tructure (NEXAFS) and X-ray photoelectron spectroscopy (XPS)) was used to study the charge state of ions in Bi2Mg1−xCoxTa2O9. The NEXAFS and XPS data showed that doping with cobalt and magnesium did not change the bismuth and tantalum oxidation states in pyrochlore; in particular, the ions maintained their oxidation states of Bi(+3), Mg(+2) and Ta(+5). The energy position of the peaks of the Ta4f-, Ta5p-, Ta4d spectra had a characteristic shift towards lower energies compared to the binding energy in pentavalent tantalum oxide Ta2O5. A shift towards lower energies is characteristic of a decrease in the effective positive charge; in particular, for the Ta4f and Ta4d spectra we presented, this energy shift was ΔE = 0.65 eV, and in the region of the Ta4d edge—0.55 eV. This in turn allowed for us to assume that tantalum atoms have the same effective charge +(5-δ). The oxidation state of cobalt ions was predominantly 2+ and partially 3+, according to NEXAFS spectroscopy data.

Mesoporous Nitrogen-Doped Holey Reduced Graphene Oxide: Preparation, Purification, and Application for Metal-Free Electrochemical Sensing of Dopamine.

Holey graphenic nanomaterials with porosity within the basal plane attract significant interest. It is observed that the perforation of graphene can enhance the specific surface area of the nanosheet, ensuring effective wetting and penetration of electrolytes to the electrode surface, facilitating rapid charge transfer, and boosting the electrocatalytic efficacy of the transducers. This study reports the first example of nitrogen-doped holey reduced graphene oxide with a mesoporous morphology of the graphene basal plane (N-MHG). It is shown that N-MHG can be synthesized through a one-step hydrothermal treatment of GO using NH3 and H2O2. A straightforward procedure for the purification of N-MHG has also been developed. AFM, TEM, and Raman analyses have revealed that N-MHG possesses a highly mesoporous network structure with a pore size ranging from 10 to 50 nm. X-ray photoelectron spectroscopy data have indicated a partial reduction of the graphene oxide sheets during the etching process but also show a 3-5 times higher content of C═O and O-C═O fragments compared to rGO. This could account for the remarkable stability of the N-MHG aqueous suspension. An electrochemical sensor for dopamine analysis is assembled on a glassy carbon electrode with N-MHG/Nafion membrane and characterized by cyclic voltammetry and electrochemical impedance spectroscopy.

Large Language Model-Informed X-ray Photoelectron Spectroscopy Data Analysis

X-ray photoelectron spectroscopy (XPS) remains a fundamental technique in materials science, offering invaluable insights into the chemical states and electronic structure of a material. However, the interpretation of XPS spectra can be complex, requiring deep expertise and often sophisticated curve-fitting methods. In this study, we present a novel approach to the analysis of XPS data, integrating the utilization of large language models (LLMs), specifically OpenAI’s GPT-3.5/4 Turbo to provide insightful guidance during the data analysis process. Working in the framework of the CIRCE-NAPP beamline at the CELLS ALBA Synchrotron facility where data are obtained using ambient pressure X-ray photoelectron spectroscopy (APXPS), we implement robust curve-fitting techniques on APXPS spectra, highlighting complex cases including overlapping peaks, diverse chemical states, and noise presence. Post curve fitting, we engage the LLM to facilitate the interpretation of the fitted parameters, leaning on its extensive training data to simulate an interaction corresponding to expert consultation. The manuscript presents also a real use case utilizing GPT-4 and Meta’s LLaMA-2 and describes the integration of the functionality into the TANGO control system. Our methodology not only offers a fresh perspective on XPS data analysis, but also introduces a new dimension of artificial intelligence (AI) integration into scientific research. It showcases the power of LLMs in enhancing the interpretative process, particularly in scenarios wherein expert knowledge may not be immediately available. Despite the inherent limitations of LLMs, their potential in the realm of materials science research is promising, opening doors to a future wherein AI assists in the transformation of raw data into meaningful scientific knowledge.

Synthesis of cerium-doped gadolinium gallium aluminum garnet (GGAG:Ce) scintillating powder via solvothermal method

The powder material Gd3Ga3Al2O12:Ce (GGAG doped with Cerium) has garnered significant attention in radiation detection due to its high light yield and rapid decay time. Despite its potential, the synthesis of high-quality and reproducible GGAG:Ce scintillating powder remains a considerable challenge. In this study, we present a solvothermal approach with an annealing temperature of 1300 °C for producing cerium-doped GGAG powder with varying concentrations (4, 2, and 0.5 mol%). The structural and luminescent characteristics were meticulously examined using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), photoluminescence (PL), radioluminescence (RL) spectroscopy, and X-ray photoelectron spectroscopy (XPS). XRD analysis confirmed the single-cubic phase garnet structure of the synthesized powder. By comparing the intermediate solvothermal products synthesized at different sintering temperatures (900 °C for 3 h and 1300 °C for 1 and 3 h), a direct correlation between solvothermal conditions and the structure/property relationships of the product was established. FESEM images revealed an ellipsoidal to irregular morphology of the as-synthesized GGAG:Ce microparticles, ranging from 0.1 to 0.3 μm, regardless of the Ce concentration. PL spectra demonstrated a strong emission peak at approximately 550 nm, characteristic of Ce3+ ions. RL data confirmed the peak luminescence at around 550 nm, with an almost twofold increase in intensity as the concentration of Ce3+ increased from 0.5 mol% to 4 mol%. XPS data disclosed the Ce3+/Ce4+ ratio in solvothermally synthesized GGAG:Ce, wherein Ce loading of 4 mol% demonstrated the increase in Ce3+ concentration to 95%, whereas the concentration of Ce4+ decreased to 5%. Notably, the highest luminescence efficiency was achieved with GGAG:Ce at a 4 mol% concentration. Thus, the solvothermal method employed in GGAG:Ce synthesis presents a straightforward approach, yielding rapid results with precise control over particle morphology and size.

Effect of metal organic framework alginate aerogel composite sponge on adsorption of tartrazine from aqueous solutions: Adsorption models, thermodynamics and optimization via Box-Behnken design

La-MOF has an excellent chance of eliminating food and industrial coloring pollutants from water because it is a typical metal-organic framework material. Nevertheless, the challenging liquid recovery has restricted the use of this powdered adsorbent. In order to solve this shortcoming, we created composite beads (La-MOF@CA aerogel composite sponge) by solidifying sodium alginate and La-MOF together. A common technique to boost an adsorbent material's adsorption capability is to modify its composition; this is especially true for adsorbents composed of metal organic framework. The effects of La-MOF@CA aerogel composite sponge on the adsorption and elimination of tartrazine (TZ) were examined in this study. Following thorough characterization, the following tests were performed: X-ray diffraction (XRD), energy-dispersive X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and Brunauer-Emmett-Teller surface area (BET). The La-MOF@CA aerogel composite sponge has a significant high surface area of 1244.68 m2/g and this surface area was decrease after adsorption of TZ to be 768.98 m2/g. the greatest adsorption capacity (qmax) of for TZ, 710.75 mg/g. Examine how the adsorption process is impacted by factors like temperature, adsorbent dosage, pH, and TZ concentration. The pHZPC was 5.18 and optimum pH for adsorption and removal of TZ was 4. The adsorption process was fitted to the pseudo-second-order equation kinetically, and to the Langmuir equation isothermally. As the adsorption energy Ea was 22.76 kJ/mol indicated that the adsorption process was chemisorption. The adsorption process was thought to be endothermic and spontaneous based on adsorption thermodynamics. The temperature increased in tandem with the amounts of materials absorbed. With good efficiency, no change in chemical composition, and similar XRD and XPS data before and after reuse, the La-MOF@CA aerogel composite sponge was reused five times. Examine the interaction mechanism between the heavy TZ and the La-MOF@CA aerogel composite sponge. Box Behnken-design was used to maximize the adsorption results (BBD).

Electronic structure of CeCu4In from band structure calculations and X-ray photoelectron spectroscopy

We present a combined new experimental and theoretical study of the electronic structure for the heavy fermion CeCu4In based on X-ray photoelectron spectroscopy (XPS) data and ab-initio band structure calculations. The compound crystallizes in the orthorhombic CeCu4.38In1.62 type of structure (space group Pnnm). Below the Fermi energy the total density of states contains mainly 3d–states of Cu atoms that hybridized with the Ce 4f electronic states. The Ce core-level XPS spectra point to a stable trivalent configuration of Ce atoms in CeCu4In, consistently with the magnetic susceptibility data. For more detailed information about electronic states the fully relativistic band structure was calculated within the density functional theory (DFT) for the first time. Based on these calculations we present calculated photoemission spectra, which very well reproduce the experimental ones. The Fermi level is located at a deep decrease in the density of electronic states and reaches a value of 3.69 states/(eV f.u.). This value is much smaller than the one obtained experimentally, which indicates the importance of many-body effects, which are not properly taken into account in ab-initio calculations. The valence band is formed mainly by Cu(3d) electrons with a small contribution of Ce(4f) electrons in the immediate vicinity of the Fermi level.

Enhancing brilliant green dye removal via bio composite chitosan and food-grade algae capsulated ruthenium metal-organic framework: Optimization of adsorption parameters by box-behnken design

A natural material made of chitosan (CS) and algae (food-grade algae, FGA) was cross-linked and loaded onto a ruthenium metal organic framework to create a bio-adsorbent (Ru-MOF@CS/FGA composite sponge) with the aim of adsorbing and eliminating Brilliant green (BG) from aqueous solutions. A range of methods were employed to analyze the Ru-MOF@CS/FGA composite sponge, such as X-ray photoelectron spectroscopy (XPS) for elemental analysis, Fourier transform infrared spectroscopy (FTIR) to ascertain the function groups, and scanning electron microscopy (SEM) to establish the surface morphology, and powder X-ray diffraction (PXRD) to study of single and multi-phase polycrystalline materials. Brunauer-Emmett-Teller surface area (BET) confirmed the adsorbent's high surface area and pore volume (826.85 m2/g and 1.28 cm3/g, respectively) and decreased to 475.62 m2/g and 0.74 cm3/g after adsorption. Determine the several factors that affect the adsorption process, such as pH, the adsorbent's dose, the initial BG concentration, and the effect of salinity. The adsorption process was fitted to pseudo-second-order kinetics and Langmuir isotherms. Dubinin-Radushkevich analysis revealed that the adsorption energy was 23.8 kJ/mol, indicating chemisorption as the mode of adsorption. It was discovered through examining the impact of temperature and computing positive-charged enthalpy and entropy that the adsorption process was endothermic, meaning that it increased in response to temperature. It is possible to reuse the Ru-MOF@CS/FGA composite sponge six times with acceptable efficiency, no change in its chemical composition, and comparable FT-IR, XPS, and XRD data before and after each reuse. Examine the mechanisms of adsorbent-adsorbate interaction, which may involve H-bonding, n-π stacking, electrostatic forces, and pore filling. The adsorption results were optimized with the Box Behnken-design (BBD).

Synthesis, XPS and NEXAFS spectroscopy study of Zn, Cr codoped bismuth tantalate pyrochlores

The study investigated the formation of inhomophase ceramics through Zn doping in Bi2СrTa2O9.5–Δ. It was found that all Bi2ZnxCr1–xTa2O9.5–Δ (0.3 ≤ x ≤ 0.7) investigated samples crystallized in the pyrochlore structural type (sp. Gr. Fd-3m) and contained an admixture of triclinic β-BiTaO4 (up to 24 wt %, sp. gr. P-1), with the admixture concentration proportional to the degree of zinc doping. It was shown that impurities in the samples could be eliminated by creating a defective bismuth sublattice proportional to the impurity content, resulting in single-phase Bi2–yZnxCr1–xTa2O9.5–Δ (y ≤ 0.5, 0.3 ≤ x ≤ 0.7) samples with the pyrochlore structure. The unit cell parameter of pyrochlore increased with an increase in zinc ion content in the samples from 10.4493 Å (x = 0.3) to 10.4976 Å (x = 0.7). The microstructure of ceramics was represented by individual slightly melted grains 0.5–2 μm in size, which increased in size and fuse with each other with an increase in zinc content. The near edge X-ray absorption fine structure (NEXAFS) and X-ray photoelectron spectroscopy (XPS) data showed that zinc doping did not change the oxidation degree of bismuth and tantalum in pyrochlore, with the ions in charge states Bi(+3), Zn(+2) and Ta(+5). The study also observed an energy shift of the absorption band in the Ta 4f spectrum toward lower energies (ΔE = 0.55 eV) characteristic of tantalum ions with an effective charge (+5–δ) and a shift of the Bi 4f7/2 and Bi 4f5/2 bands shift to lower energies with increase in x(Zn), due to the distribution of some Zn(II) ions in the bismuth position. The oxidation degree of chromium ions in the samples was mainly (+3), with some chromium ions oxidized and having an oxidation degree close to (+6) according to NEXAFS data. The studied ceramics showed promise as dielectrics for multilayer ceramic capacitors and devices for microwave applications due to their low sintering temperature and high porosity.

Investigating the mechanism of formation of Ca-rich Ca[sbnd]Yb apatite that forms from the Yb-silicate–CMAS reaction at 1300°C

The formation mechanism and structure of Ca-rich CaYb apatite, which forms from the corrosion of Yb-silicate based coatings with CMAS at 1300°C in air for 48 h was investigated. X-ray photoelectron spectroscopy (XPS) was used to determine the bond type and oxidation states of the apatite. XPS data showed that the Si2p peaks are related to silicates, while the Ca2p and Yb4d are linked to apatite structures. The mechanism of growth for the apatite is proposed using the Wagner-Hauffe oxidation principle and the Kröger-Vink notations. The formation mechanism of the apatite-structure reaction phase is by substitutional diffusion, which is governed by the movement (formation and destruction) of point defects within the Yb2O3 lattice, particularly oxygen vacancies and electron holes. When Ca2+ substitutes Yb3+ in its lattice position, this results in the formation of anionic vacancies, which leads to more Ca2+ diffusion. The diffusion process continues until vacancies can no longer form to achieve electroneutrality, which leads to the newly formed Yb–Ca–Si being saturated with cations. Thus, based on this investigation, it is assumed that a CaYb silicate oxyapatite coatings can suppress the vacancy formation mechanism by containing high Ca and Si content which can thus decrease the ionic diffusion from CMAS melt into the EBC lattice. This can be the premises of a more CMAS-resistant coating family.

Harmonic amide bond density as a game-changer for deciphering the crosslinking puzzle of polyamide

It is particularly essential to analyze the complex crosslinked networks within polyamide membranes and their correlation with separation efficiency for the insightful tailoring of desalination membranes. However, using the degree of network crosslinking as a descriptor yields abnormal analytical outcomes and limited correlation with desalination performance due to imperfections in segmentation and calculation methods. Herein, we introduce a more rational parameter, denoted as harmonic amide bond density (HABD), to unravel the relationship between the crosslinked networks of polyamide membranes and their desalination performance. HABD quantifies the number of distinct amide bonds per unit mass of polyamide, based on a comprehensive segmentation of polyamide structure and consistent computational protocols derived from X-ray photoelectron spectroscopy data. Compared to its counterpart, HABD overcomes the limitations and offers a more accurate depiction of the crosslinked networks. Empirical data validate that HABD exhibits the expected correlation with the salt rejection and water permeance of reverse osmosis and nanofiltration polyamide membranes. Notably, HABD is applicable for analyzing complex crosslinked polyamide networks formed by highly functional monomers. By offering a powerful toolbox for systematic analysis of crosslinked polyamide networks, HABD facilitates the development of permselective membranes with enhanced performance in desalination applications.