X-ray Diffraction Spectroscopy Research Articles

X-ray Characterizations of Exfoliated MoS2 Produced by Microwave-Assisted Liquid-Phase Exfoliation

An X-ray analysis of exfoliated MoS2, produced by means of microwave-assisted liquid-phase exfoliation (LPE) from bulk powder in 1-methyl-2-pyrrolidone (NMP) or acetonitrile (ACN) + 1-methyl-2-pyrrolidone (NMP) solvents, has revealed distinct structural differences between the bulk powder and the microwave-exfoliated samples. Specifically, we performed X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) measurements to identify the elements of our exfoliated sample deposited on a Si substrate by drop-casting, as well as their chemical state and its structural crystalline phase. In the exfoliated sample, the peaks pattern only partially resemble the theoretical Miller indices for MoS2. In contrast, the bulk powder’s spectrum shows the characteristic peaks of the 2H polytype of MoS2, but with some broadening. Notable is the retention of partial crystallinity in the post-exfoliation phases, specifically in the normal-to-plane orientation, thus demonstrating the effectiveness of microwave-assisted techniques in producing 2D MoS2 and attaining desirable properties for the material. XPS measurements confirm the success of the exfoliation procedure and that the exfoliated sample retains its original structure. The exfoliation process has been optimized to maintain the structural integrity of MoS2 while enhancing its surface area and electrochemical performance, thereby making it a promising material for advanced electronic and optoelectronic applications ranging from energy storage to sensing devices under ambient conditions.

CF3-Substituted Ethylene Carbonates for High-Voltage/High-Energy Rechargeable Lithium Metal-LiNi0.8Co0.1Mn0.1O2 Batteries.

The development of advanced liquid electrolytes for high-voltage/high-energy rechargeable Li metal batteries is an important strategy to attain an effective protective surface film on both the Li metal anode and the high-voltage composite cathode. Herein, we report a study of two CF3-substituted ethylene carbonates as components of the electrolyte solutions for Li metal|NCM811 cells. We evaluated trifluoromethyl ethylene carbonate (CF3-EC) and trans-ditrifluoromethylethylene carbonate Di-(CF3)-EC as cosolvents and additives to the electrolyte solutions. Using CF3-substituted ethylene carbonates as additives to a fluoroethylene carbonate (FEC)-based electrolyte solution enables improved capacity retention of high-power Li metal|NCM811 cells. The composition of the products from the transformations of CF3-EC and Di-(CF3)-EC in Li|NCM811 cells was studied by FTIR, XPS, and 19F NMR spectroscopy. We concluded that fluorinated Li alkyl carbonates are the main reaction products formed from these cyclic carbonates during the cycling of Li|NCM 811 cells, and fragmentation of the ring with the formation of CO2, CO, or olefins is not characteristic of CF3-substituted ethylene carbonates. The NCM 811 cathodes and Li metal anodes were characterized by X-ray diffraction, SEM, XPS, and FTIR spectroscopy. The role of CF3-substituted ethylene carbonate additives in stabilizing high energy density secondary batteries based on Li metal anodes was discussed. A bright horizon for developing sustainable rechargeable batteries with the highest possible energy density is demonstrated.

Structural phase transition, relaxor behavior, and ultra-low strain hysteresis in BaTiO3 ceramics modified by BiYO3

In this study, the structural properties, phase transition, relaxor behavior, and strain properties of (1−x)BaTiO3‒xBiYO3 (x= 0.02‒0.15 mol) ceramics were investigated. The room temperature x-ray diffraction and Raman spectroscopy results reveal that (1−x)BaTiO3‒xBiYO3 ceramics undergo phase transition from tetragonal to pseudo-cubic structure with x increasing. The curves of dielectric constant and loss tangent as a function of temperature and frequency show that the dielectric constant was changing from being dependent on temperature to being independent of it upon increasing BiYO3 amount, which is induced obvious dielectric relaxation behavior. Slimmer polarization–electric field (P–E) loops and lower remnant polarization (Pr ) were observed for samples with x ⩾ 0.08. The transition between the ferroelectric and relaxor states leads to the narrow strain–electric field (S–E) loops, which exhibit a high electric field-induced strain of 0.192% and an ultra-low strain hysteresis of 10.4% at an electric field of 70 kV cm−1 for x= 0.04. This excellent performance indicates that 0.96BaTiO3‒0.04BiYO3 ceramic may be promising lead-free materials for high-precision displacement actuators applications.

Phase engineered enhancement of photocatalytic and Opto-magnetic properties of CuO nanoparticles through fluorine and gadolinium doping

The present study comprises co-doping of CuO nanoparticles with gadolinium (Gd) and fluorine (F) using the sol-gel method to achieve phase stabilization and tune their physicochemical properties. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analyses revealed successful incorporation of the dopants and the stabilization of the CuO phase with increasing Gd content. Morphological studies revealed grain refinement and an enhanced surface-to-volume ratio upon co-doping. Average particle size decreased from 194 nm to 138 nm for pure and 5%F to 126 nm, 101 nm, and 81 nm for, 1mol%, 2mol% and 3mol% Gd along with 5mol% F co-doped CuO nanoparticles. Increasing the Gd ratio also tuned the band structure and significantly improved the optical properties of the CuO nanoparticles. Additionally, a transition from weak ferromagnetic ordering to paramagnetic behavior is observed. Coercivity decreased to 2.5 Oe for Cu0.97Gd0.03F0.05O0.95 as opposed to 396.3 Oe for CuF0.05O0.95. Photocatalytic activity studies using rhodamine B (Rh B) as a model probe revealed a pronounced enhancement in degradation kinetics with increasing gadolinium (Gd) doping, culminating in around 2.9 times faster degradation rate for 3 % Gd-doped CuO nanoparticles compared to pure CuO nanoparticles. After 3 h of UV light irradiation, the photodegradation efficiency of Cu0.97Gd0.03F0.05O0.95 was 94 %, which is significantly higher than the 80 % and 69 % efficiency of CuF0.05O0.95 and CuO, respectively. These remarkable optical, magnetic, and photocatalytic properties of the co-doped nanoparticles offer promising candidacy for various applications, including photocatalysis, solar energy harvesting, magnetic switching, and magnetic sensing.

Biosynthesis of microrubble-shaped nanoporous Co3O4/rGO NCs using leaves extract of Neolamarckia cadamba and its antibacterial/antioxidant performance

Nowadays, the whole globe is paying great attention for the sustainable development, eco-friendly and economical production of nanostructures materials. With this motivation, the present work portrayed one-step ‘in-situ’ bioinspired green fabrication of Co3O4–reduced graphene oxide nanocomposites (Co3O4–rGO NCs) for the first time utilizing an aqueous leaf extract of Neolamarckia cadamba. As-fabricated NCs were characterized by several analytical and electron microscopic techniques viz. X-ray diffraction (XRD), Fourier Transform-Infrared (FT-IR), Energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), BET (Brunauer-Emmett-Teller), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) to evaluate their phases, structure, shape, composition, chemical state, porosity, optical and morphological aspects. The XRD study revealed a cubic spinel symmetry of NCs, while crystallite size estimated around 25 nm. TEM spectroscopy exposed an average particle size 8–10 nm of Co3O4 grown on the surface of reduced graphene oxide (rGO NCs), whereas SEM analysis showed sharped microrubble-shaped morphology. The formation of NCs by doping metal oxide with rGO through in-situ method were confirmed by XRD, EDS, Raman, and XPS spectroscopy. The BET study estimated the specific surface area and pore size of NCs as 98 m2/g and 8.9 nm respectively. The Co3O4–rGO NCs demonstrated an effective bactericidal activity against S. aureus, E. coli, K. pneumoniae, and B. subtillis. Prominently it was found that, a significant antibacterial activity seen against E. coli and S. aureus at a concentration 0.1 mg/100 µL may be due to scaffold morphology, nanoscale-structures and nanoporosity of the NCs. Due to receiving significant antibacterial activity, material’s molecular docking was assessed. Furthermore, an antioxidant activity of leaf extract and NCs was evaluated by DPPH method. An outstanding biological study of bioinspired NCs revealed that material could be used as a potent antimicrobial agent.

Development of a glycine-MWCNT nanohybrid via electropolymerization for enhanced electrochemical detection of diclofenac

In this study, electropolymerization of glycine (Gly) was carried out to enhance the sensitivity of the carbon paste electrode (CPE) blended with multi-walled carbon nanotubes (MWCNTs) for electroanalysis of diclofenac (DCF). Analytical applications and electrochemical performance were examined using various voltammetric methods, including differential pulse voltammetry and cyclic voltammetry. Atomic force, scanning electron microscopy, dispersive X-ray, X-ray diffraction, and Raman spectroscopy were used to ascertain the surface topology of the modifier. The modified sensor with high electrocatalytic properties could electrochemically oxidize DCF, resulting in an enhanced current compared to the bare CPE when an anodic peak was detected at 0.77 V peak potential for the bare CPE, consisting of 0.1 mM DCF and 2.11 µA peaks current. The working electrode CPE was then modified with MWCNT and glycine. For MWCNT/CPE, a peak was seen at 5.20 µA and 0.75 V, and a more intense peak was observed for poly(Gly)-MWCNT/CPE at 11.52 µA and 0.74 V. The poly(Gly)-MWCNT/CPE exhibited a five-fold enhancement of peak current compared to bare CPE. The modified electrode displayed fast electron transfer, reproducibility, and repeatability. The study explored how factors like immersion time, pH variation, scan speed, and substance concentration could influence the peak current of DCF. Methods such as differential pulse voltammetry and cyclic voltammetry were utilized to examine the electrochemical oxidation behavior of DCF. The concentration variation is 0.5 µM to 7.0 µM, and the detection limit was 7.96 × 10-8 M. The rate constant (ks) for the electrochemical process was 1.710 s-1. The DCF of pharmacological and biological test substances was measured using the constructed modified electrode.

Ligand Noninnocence in β-Diketiminate and β-Diketimine Copper Complexes.

Metal-ligand cooperative systems have a long precedent in catalysis, with the classification depending on the site of substrate bond cleavage and formation and on redox state changes. Recently, our group reported the participation of a β-diketiminate ligand in chemical bonding to heterocumulenes such as CO2 and CS2 by tricopper complexes, leading to cooperative catalysis. Herein, we report the reactivity of these copper clusters, [Cu3EL]- (E = S, Se; L = tris(β-diketiminate) cyclophane ligand), toward other electrophiles, viz. alkyl halides and Brønsted acids. We identified a family of ligand-functionalized complexes, Cu3EL (R) (R = primary alkyls), and a series of disubstituted products, Cu3EL (R)2, through single-crystal X-ray diffraction, mass spectrometry, and infrared and UV-visible spectroscopy. As part of mechanistic studies on these alkylation reactions, we evaluated the acid-base reactivity of these complexes and the influence of the backbone substitution on the reduction potential. Implications of these findings for ligand noninnocence and the relevance of the metal core as a cofactor for the ligand's reactivity are discussed.

Promoted stability of Cu/ZnO/Al2O3 catalysts formethanol production from CO2 hydrogenation by La modification

Deactivation of Cu/ZnO/Al2O3 catalysts in CO2 hydrogenation to methanol reaction is one of the main reasons limiting their application. We synthesized a series of La modified Cu/ZnO/Al2O3 catalysts by adding different contents of La to improve the stability. In the 100 h short-term stability test at 200 °C under 3 MPa with a GHSV of 12000 mL/(g·h), the unmodified Cu/ZnO/Al2O3 catalysts degraded obviously over 100 h. In sharp contrast, the stability was significantly promoted by the addition of La. The best activity was achieved with 5% La added samples (4% CO2 conversion and 85% methanol selectivity),which also showed impressive stability over 1000 h except about 17% deactivation during the initial 190−220 h. The X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) results revealed that the addition of 5% La improved the dispersion of Cu and Zn, inhibited the sintering of Cu, stabilized the Cu0/+ species and retarded oxidation of Cu in catalysts, which attributed to the high stability of the catalysts.

Study on mechanical properties and damage mechanism of alkali-activated slag concrete

The cement industry has become one of the important sources of greenhouse gas emissions, and the alkali-activated slag (AAS) has the same mechanical properties and lower carbon emissions as cement in the production process. Therefore, it can be used as an alternative binder for low-carbon buildings. The effect of alkali concentration (mass ratio of Na2O to binder) on the macro-mechanical properties and meso-damage mechanism of alkali-activated slag concrete (AASC) under uniaxial compression was investigated in this work. Six kinds of concrete with alkali concentration of 2%, 4%, 6%, 8%, 10% and 12% were prepared. The microscopic characteristics of AASC were characterized by nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), x-ray diffraction (XRD) and x-ray energy dispersive spectroscopy (EDS); the meso-damage evolution mechanism of AASC was discussed by statistical damage theory. The results showed that the peak stress and elastic modulus of AASC specimens increased, and the microstructure became denser with the increase of alkali concentration. However, the mechanical properties of the specimen deteriorated to some extent when the alkali concentration exceeded 6%; for example, the peak stress decreased by 24.00 MPa when the alkali concentration was increased from 6% to 12% at the age of 28d. Based on the statistical damage theory, the effective stress concept was introduced to quantitatively analyze the mesoscopic damage evolution of AASC. Both fracture and yielding damage modes were considered. By exploring the regular changes of the mesoscopic parameters, the connection between the macroscopic mechanical properties and the mesoscopic damage mechanism was established. Based on the above mechanical properties and mesoscopic damage results, the alkali concentration of 6% can be used as the best mixture proportions of AASC.

Preparation of starch-based green nanofiber mats for probiotic encapsulation by electrospinning.

In this study, starch-based nanofiber mats were successfully prepared from aqueous solution by electrospinning and used for probiotic encapsulation for the first time. The physicochemical properties of the octenylsuccinated (OS) starch/poly(vinyl alcohol) (PVA) blend solutions were systematically investigated. Through Fourier transform infrared spectroscopy and X-ray diffraction spectra analysis, it was found that miscibility and hydrogen bonding interactions exist between OS starch and PVA molecules. Thermogravimetric analysis and derivative thermogravimetric analysis revealed that the produced nanofibers possess satisfactory thermal stability. Scanning electron microscopy images and diameter distribution histograms showed that continuous and defect-free nanofibers were obtained and along with the increase in the weight ratio of OS starch, the average diameter gradually decreased. In addition, it was confirmed that the probiotics were successfully encapsulated in nanofiber mats. The survival rates of Lactobacillus plantarum AB-1 and Lactobacillus rhamnosus GG encapsulated in nanofibers were as high as 94.63% and 92.42%, respectively, significantly higher than those of traditional freeze-drying. Moreover, compared to free cells, probiotics encapsulated in nanofiber mats retained better viability after 21 days of storage at 4 and 25°C, and showed remarkably higher survival rates after exposure to simulated gastric and intestinal fluid. This study showed that the developed nanofibers can be a promising encapsulation system for the protection of probiotics.

Evolution of macromolecular structure during coal oxidation via FTIR, XRD and Raman

The analysis of the macromolecular structure and morphology in coal during oxidation is the basis to explore the mechanism of spontaneous combustion. To explore the evolutionary rules of coal macromolecular structure during oxidation, Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), and Raman Spectroscopy (Raman) were employed to analyze the coal samples with different oxidation degrees. The results revealed that the oxidation action led to the decrease of the aliphatic structures and aromatic hydroxyl groups in coal, while promoting the formation of oxygen-containing functional groups and aromatic structures. It also led to a relative increase of free hydroxyl groups linked to hydrogen bonds. The aromatic layer spacing (d002) decreased with increasing oxidation degree, while the microcrystal stacking height (Lc), the aromatic layer diameter (La), the average number of crystal stacking layers (n) generally increased. It indicated that small aromatic ring molecules in coal could undergo continuous polymerization during oxidation to form a single aromatic layer structure. The variation of Raman spectrum parameters exhibited a consistent decreasing trend in WD/WG, ID/IG, AD/AG, and A(GR+SL)/AG value, indicating an increase in the vibration of sp2 hybridization carbon atoms within the lattice structure of coal. Conversely, PG-D, AS/AD and A(GR+VL+VR)/AD value increased overall, suggesting that small aromatic rings decreased in content during oxidation while polymerizing into larger aromatic rings. The coal structure underwent a brief stage of disordered evolution during oxidation, followed by removal of impurity structures and condensation of aromatic structures due to increasing oxidation temperatures, ultimately leading to a highly ordered crystalline state. The oxidation process significantly influenced the development of coal's aromatic structure, particularly in less metamorphic coal. The research findings provide a theoretical basis for analyzing the underlying mechanism behind spontaneous combustion induced by coal oxidation.

Enhancement of the environmental stability of perovskite thin films via AZ5214-photoresist and PMMA coatings

This study presents a novel investigation into enhancing the environmental stability of perovskite thin films, specifically focusing on the effects of AZ5214 photoresist compared to the widely studied PMMA. By employing advanced matrix encapsulation techniques, we aim to stabilize methylammonium lead iodide (MAPbI3) and methylammonium lead bromide (MAPbBr3) films, which are meticulously prepared via a two-step solution deposition method under controlled ambient conditions. Our approach involves spin-coating layers of poly(methyl methacrylate) (PMMA) and AZ5214 photoresist to singularly encapsulate the perovskite films. This encapsulation provides a robust hydrophobic barrier, significantly mitigating moisture ingress and addressing pinhole challenges within the perovskite structure. Through comprehensive characterizations—including scanning electron microscopy (SEM), X-ray diffraction (XRD), and photoluminescence (PL) spectroscopy—we demonstrate that AZ5214 photoresist, despite being thicker than PMMA, offers significantly enhanced stability. Our study revealed that coating MAPbI3 perovskite with a 127-nanometer layer of PMMA resulted in a PL intensity retention of 44.8% after 40 days, which is a 589.23% improvement over the uncoated perovskite. Similarly, a 1200-nanometer layer of AZ5214 photoresist achieved a PL intensity retention of 38.2%, reflecting a 487.69% enhancement. For MAPbBr3 perovskite, the PMMA coating achieved a PL intensity retention of 43.1%, a 71.72% improvement, while the AZ5214 photoresist coating resulted in a retention of 48.4%, showing a 92.83% enhancement. These findings highlight the superior stability provided by AZ5214 photoresist, especially for MAPbBr3, making it a more effective barrier against environmental degradation compared to PMMA.

Molybdenum and Vanadium-Codoped Cobalt Carbonate Nanosheets Deposited on Nickel Foam as a High-Efficient Bifunctional Catalyst for Overall Alkaline Water Splitting

To address issues of global energy sustainability, it is essential to develop highly efficient bifunctional transition metal-based electrocatalysts to accelerate the kinetics of both the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER). Herein, the heterogeneous molybdenum and vanadium codoped cobalt carbonate nanosheets loaded on nickel foam (VMoCoCOx@NF) are fabricated by facile hydrothermal deposition. Firstly, the mole ratio of V/Mo/Co in the composite is optimized by response surface methodology (RSM). When the optimized composite serves as a bifunctional catalyst, the water-splitting current density achieves 10 mA cm−2 and 100 mA cm−2 at cell voltages of 1.54 V and 1.61 V in a 1.0 M KOH electrolyte with robust stability. Furthermore, characterization is carried out using field emission scanning electron microscopy-energy dispersive spectroscopy (FESEM-EDS), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). Density functional theory (DFT) calculations reveal that the fabricated VMoCoCOx@NF catalyst synergistically decreases the Gibbs free energy of hydrogen and oxygen-containing intermediates, thus accelerating OER/HER catalytic kinetics. Benefiting from the concerted advantages of porous NF substrates and clustered VMoCoCOx nanosheets, the fabricated catalyst exhibits superior electrocatalytic performance. This work presents a novel approach to developing transition metal catalysts for overall water splitting.

NiO/vermiculite composites prepared for photocatalytic degradation of methanol-water solution and hydrogen generation

A novel eco-friendly NiO/Vm clay based photocatalysts were synthesized from two vermiculites (Vm1 and Vm2) and nickel(II) nitrate hexahydrate (Ni(NO3)2·6H2O salt precursor by the chemical precipitation without and with the sodium hydroxide (NaOH) or ammonium hydroxide (NH4OH, 28% NH3 in H2O) as precipitation agents (Synthesis A) in comparison with the solid-state thermal decomposition (Synthesis B) at 600 °C. Structural properties of all specimens were characterized by X-ray fluorescence, scanning electron microscopy, X-ray diffraction, infrared (IR) and Raman spectroscopy. The photocatalytic performance of NiO/Vm composites was evaluated under UV radiation (λ = 254 nm) for decomposition of methanol-water to hydrogen over 4-h and the stable yield of hydrogen over the 24-h periods. The NaOH and NH4OH affected the NiO crystallite size and therefore the photocatalytic activity during 4 h. Different 2:1 layer charge of Vm1 (0.82 e−) and Vm2 (0.40 e−) and the specific surface area of Vm1 (about 43 m2/g) and Vm2 (about 34 m2/g) supported H2 yield of 628.2 μmol/gcat. and 596.8 μmol/gcat., close to 657.0 μmol/gcat. produced in the presence of commercial photocatalyst TiO2 Evonik P25. Crystalline NiO precipitated and anchored in NiO/Vm composites contained smaller crystallites than those in free NiO. Vermiculite silica surface supports coverage of NiO by hydrogen bonding to Si-OH groups influencing the geometry of the NiO crystal structure (disorder NiO(X)). The heterojunction with Si-O-Ni bonding, at which electrons transfer from Vm to NiO cause enriching electron density in NiO and favoring its photocatalytic activity. Photocatalytic hydrogen generation from methanol–water mixture at the presence of all specimens indicated the main product H2 and minimum by-products CH4 and CO. The stable hydrogen production for 24 h was confirmed only in the presence NiO/Vm1–24 while maintaining the NiO(X) in small crystallites. The thermal solid-state procedure provided the gradual dehydration of vermiculites and Ni(NO3)2·6H2O to the same amount and crystallinity of NiO in NiO/Vm1 and NiO/Vm2 composites. The results of this work confirm that vermiculites mixed layer structures with different negative layer charge play a dominant role as semiconductors for anchored NiO. The photocatalytic activity of NiO/vermiculite composites can be harnessed to treat wastewater containing organic contaminants.

One stone, three birds: Cu2+-substituted chloride electrolyte for high-performance all-solid-state lithium batteries

Emerging solid electrolytes, represented by Li2ZrCl6 (LZC), hold great potential due to their lower costs and superior electrochemical stability compared to sulfide SEs (e.g. Li5.4PS4.4Cl1.6). However, challenges such as relatively low ionic conductivity and instability with lithium hinder its widespread application. This work develops a cost-effective strategy by substituting Cu2+ for Zr4+ in LZC electrolyte. The evolution of electrolyte structure at varying substitution levels is comprehensively investigated by synchrotron X-ray diffraction and Raman spectroscopy. The optimized Cu2+-substituted LZC achieves a notable ionic conductivity of 0.75 mS cm−1 due to a reduced energy barrier for Li+ migration confirmed by first-principles calculations. Symmetric lithium cells with the Cu2+-substituted LZC exhibit enhanced inhibition to lithium dendrites than those with Li5.4PS4.4Cl1.6. X-ray photoelectron spectroscopy unveils the key role of Cu2+ reduction in the inhibition of the lithium dendrite, enabling the cell to stably cycle at 0.5 mA cm−2. Moreover, the Cu2+-substituted LZC exhibits improved electrochemical stability, marked by small anodic current exceeding 4 V, reduced polarization, and rapid lithium-ion diffusion kinetics. All-solid-state batteries fabricated with the Cu2+-substituted LZC and Li/LiNi0.8Mn0.1Co0.1O2 electrodes present a high reversible capacity of 139.2 mAh g−1 with retention rate of 96.9 % after 200 cycles at 0.5 C.

Biosynthesized and chemically synthesized Ag/TiO2 nanocomposites: Effect of reaction parameters on synthesis using watermelon rind extract and comparative analysis

This work synthesized Ag/TiO2 nanocomposite via an aqueous reduction method using a green and chemical reducing agent. Citrullus lanatus (watermelon) rind extract (WMRE) and sodium borohydride (NaBH4) were used as the reducing agents during green synthesis and chemical synthesis, respectively. During green synthesis, a pH of 12, a reaction time of 45 min, and an operating temperature of 100 °C yielded the best visible light activity. The biosynthesized and chemically-synthesized Ag/TiO2 were compared using UV–Vis spectroscopy, X-ray fluorescence spectroscopy (XRF), X-ray diffraction spectroscopy (XRD), Fourier transform infrared spectroscopy (FTIR), energy dispersive spectroscopy-scanning electron microscopy (EDS-SEM) and transmission electron microscopy (TEM). Synthesis using WMRE yielded spherical Ag nanoparticles modified on the surface of TiO2 nanoparticles. The Ag nanoparticles had enhanced monodispersity with an average diameter of 7.48 ± 4.06 nm. Therefore, the developed WMRE green synthesis method provides a simple, less chemical-intensive, and effective alternative to chemical synthesis.

Facile one-step synthesis and characterization of MnO nanoneedles and their application in solar photocatalysis

Manganese oxide (MnO) colloidal nanoneedles have been successfully synthesized by a facile one-step method based on the alkaline reaction of the precursor manganese acetate salt and excess sodium hydroxide. X-ray diffraction and FT-IR spectroscopy confirmed the synthesized MnO nanoneedles phase and structure. The optical properties of synthesized MnO nanoneedles were studied by UV–Vis absorption spectroscopy. Optical particle size and band gap of synthesized MnO colloidal nanoneedles were calculated. HR-TEM/SEM images and EDX allow us to determined particle shape and size. The photocatalytic activity of the MnO nanoneedles was evaluated using the Congo red azo dye in an aqueous solution under solar light irradiation. The results showed that nanoneedles, compared with commercial ZnO nanoparticles, exhibited high photocatalytic activity. The photocatalytic studies also showed that various parameters such as band gap, size, shape, and rate constant velocity remarkably affected the remotion rate of Congo red azo dye.

Rare earth mixed sandwich complexes with tetraalkylphospholide and cyclooctatetraenide ligands

A series of rare earth (mono)phospholide mixed sandwich complexes of the general form [M(PC4R4)(COT)(THF)n] (M = Sc, Y, La, Lu; R = Me, Et; COT = cyclooctatetraenide, {C8H8}2–; n = 0 to 2) have been isolated by the treatment of iodide precursors, [M(COT)(I)(THF)n], (1M, M = Sc, Y, Lu, n = 2; M = La, n = 3) with potassium phospholide salts, [K(PC4R4)]n (R = Me, Et). The solid-state molecular structures and speciation of these sandwich complexes depends upon both the ionic radius of the rare earth metal, along with small steric and solubility differences which arise between the two per-alkylated phospholide ligands. The smaller {PC4Me4} ligand gave monomeric Lewis-base free [M(C8H8)(PC4Me4)] (2M, M = Sc, Lu) with smaller rare earths Sc(III) and Lu(III), but moving to larger ions Y(III) and La(III), the products were poorly soluble and could only be isolated as THF-adducts, [Y(C8H8)(PC4Me4)(THF)] (3) and [La(C8H8)(PC4Me4)(THF)2] (4). The slightly increased steric demands of {PC4Et4} gave monomeric Lewis-base free complexes for Sc(III), Lu(III), and Y(III) in [M(C8H8)(PC4Et4)] (5M, M = Sc, Y, Lu), whereas for La(III) a dimeric complex was isolated, [La(C8H8)(µ-PC4Et4)]2 (6). We also report the synthesis and molecular structures of 1Sc and 1Lu, as well as [LuI3(THF)3] (7) for the first time. All complexes were characterised by single crystal X-ray diffraction, multi-nuclear NMR, UV-Vis-NIR and ATR-IR spectroscopies in addition to elemental analysis.

Hydrothermally synthesized Ag2Te on metallic 2D templates

Silver telluride, Ag2Te, was synthesized on various 2D templates of carbon nanotubes (CNT) and transition-metal dichalcogenides (WTe2 and VTe2) via hydrothermal synthesis. X-ray diffraction (XRD) and Raman spectroscopy revealed that Ag2Te was synthesized on the 2D templates under optimal synthesis conditions. Differential scanning calorimetry (DSC) confirmed that the structural phase transition of Ag2Te underwent endothermic and exothermic reactions at approximately 410 and 425 K, respectively. Among various metallic templates, a large amount of Ag2Te has been synthesized on strongly acidic CNT. X-ray absorption near-edge structure (XANES) revealed that the chemical state of the metallic support influenced the electronic structure of the as-grown Ag2Te on the metallic supports. Our findings demonstrated that the hybrid 2D catalysts with an appropriate 2D metallic template can be a promising strategy for achieving efficient catalysis.

Effect of Ce on structural evolution and corrosion resistance of HRB500E rebar corrosion layer

HRB500E rebar is a low-alloy high-strength steel with excellent mechanical properties and good plasticity but suffers from deficient corrosion resistance. This can be solved by adding trace elements, including rare earth elements. Herein, the corrosion-resistant behavior of rebar was evaluated by weightlessness testing and electrochemical measurements, and the effects of Ce on the structural evolution of the corrosion product layer were investigated by scanning electron microscopy (SEM), Electron Probe X-ray Micro-Analyzer (EPMA), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). The results showed that adding Ce to the rebar improved the densification of the reinforcing surface corrosion products, as well as reduced the corrosion rate of the experimental rebar. Compared to C0 sample without Ce, the rebar sample containing 0.044 wt.% Ce displayed increased Ecorr by 0.051 V, decreased Icorr by 15.573 mA cm−2, enhanced Rc of the corrosion product layer by 112.71 Ω cm2, incremented α-FeOOH content in the corrosion product layer, and boosted ratio of α/γ* in the corrosion product layer by 10.11%. Furthermore, the oxide (CeO2) formed by Ce in the corrosion layer of the rebar bar surface existed in the rust layer, resulting in a stable corrosion product layer with improved blocking ability of the corrosive medium. Overall, the addition of Ce at certain ratios looks promising to produce HRB500E rebar with excellent corrosion resistance and extended service life under harsh conditions.