Energy Dispersive X-ray Absorption Research Articles

Tracking Minority Species in Redox Reactions: A Quantitative Combined XAS and Modulation Excitation Study.

Understanding the nature of intermediates/active species in reactions is a major challenge in chemistry. This is because spectator species typically dominate the experimentally derived data and consequently active phase contributions are masked. Transient methods offer a means to bypass this difficulty. In particular, modulation excitation with phase-sensitive detection (ME-PSD) provides a mechanism to distinguish between spectator and reacting species. Herein, modulation excitation (ME) time-resolved (energy dispersive) X-ray absorption spectroscopy, assisted by phase sensitive detection (PSD) analysis, has been applied to the study of a liquid phase process; in this case the classic ferrocyanide/ferricyanide redox couple. Periodic switches of the electrical potential (anodic/cathodic) enabled the use of the ME approach. Structural changes at fractions as low as 2 % of the total number of electroactive species were detected within the X-ray beam probe volume containing ~30 pmol of Fe(II)/Fe(III).

Engineering of Soft Urea Synthesized Ni3n Nanomaterials for Oxygen Evolution Reaction

Most active electrocatalysts include platinum-group metals (PGMs) and their alloys for electrochemical water splitting, but they are strongly limited by material cost and scarcity. [1] On the other hand, transition metal nitrides overcome this bottleneck and show high electrical conductivity, making them catalytically active for water electrolysis. The high conductivity is based on the incorporation of nitrogen atoms into the unit cell of metal, leading to their d-band contraction with electron density enhancement below Fermi level. [2] For instance, metallic nickel nitride (Ni3N) has been widely reported as a promising electrocatalyst material to accelerate the oxygen evolution reaction (OER) by in-situ forming a nickel (oxy)hydroxide [Ni(OH)2 and NiOOH] layer. [3] The Ni3N materials can be prepared by single step soft-urea route to obtain pure crystal phase [4] or a composite with carbon [5], which rises the following two research questions: 1. What are the optimal synthesis parameters of the soft-urea route to control the structure of Ni3N? 2. What is the relationship between structure and OER activity for Ni3N materials?In this work, we used the soft-urea route to prepare Ni3N materials by varying the ratios of NiCl2, urea and ethanol as precursor chemicals. The precursors were made into a gel by magnetic stirring having metal:urea ratio of 1:5, and then heated up to 400 ºC in a tubular furnace with constant flow of argon. The as-prepared Ni3N were then characterized by X-ray diffraction (XRD), elemental analysis (CHN), transmission electron microscopy (TEM) equipped with an energy-dispersive X-ray spectroscopy (EDX) and X-ray absorption spectroscopy (XAS).Based on the quantitative Rietveld refinement, the formation of pristine Ni3N materials is strongly controlled by the annealing temperature. In addition to the Ni3N phase, we observed the formation of the fcc Ni phase (0 – 10 wt.%) as a minor phase. The TEM images show individual particles of below 100 nm in size. Rotating disc electrode (RDE) technique was employed to establish the electrochemical OER activity of Ni3N materials by sweeping the potential from 1.3 to 1.8 VRHE at 10 mV s-1 in Ar-saturated 0.1 M KOH. Polycrystalline Ni and Ni particles are taken as reference materials. We observed an improvement of the OER activity as the overpotential at 10 mA cm-2 (normalized by the geometric surface area) reduced from 379 mV (poly-Ni) to 358 mV (Ni3N). Furthermore, in-situ XAS studies were performed to better understand the nature of the redox reactions between Ni species and the in-situ formation of nickel (oxy)hydroxide [Ni(OH)2 and NiOOH] layers before and during the OER as a function of the applied potential. Based on the in-situ XANES data, we correlated the structure of Ni3N/fcc-Ni/carbon composite with observed OER activity under alkaline conditions.To summarize, we were able to prepare a composite of Ni3N/fcc-Ni/carbon material with improved OER activity via soft-urea route. The in-situ formation of the layered nickel (oxy)hydroxide [Ni(OH)2 and NiOOH] layers as the catalytically active OER species were probed by in-situ XANES data.

Solution combustion synthesis and exploration of chromium reduction and organic dyes degradation of cobalt tungstate (CoWO4) nanoparticles

Facile preparation route for cobalt tungstate (CoWO4) via cost effective, time saving, easy and solution combustion approach is described in the present paper. The structural, morphological properties of cobalt tungstate characterized by different physiochemical techniques which include X-ray diffraction, scanning electron microscopy (SEM), energy dispersive X-ray absorption (EDS). The optical properties assessed by UV–visible spectroscopy (DRS) and photoluminescence spectroscopy (PL). Using these methods, it was discovered that CoWO4 which has been synthesized displayed a monoclinic phase of Wolframite with great crystallinity and purity. The average crystallite size of prepared CoWO4 was 22 nm and band gap obtained was 2.84 eV due to which it can be used as visible light photocatalyst in aqueous medium. As a result, in this study, the photocatalytic degradation ability of CoWO4 was assessed by observing the aqueous phase degradation of the most widely used dyes, methylene blue (MB) and Rhodamine-B as well as Cr(VI) reduction under visible light. Almost all MB degraded in 90 min whereas 69 % degradation of RhB takes place in 240 min under visible light irradation. The different aspects for low rate of photodegradation of RhB dye than MB dye was also discussed in this report. The present study deals advanced approach that CoWO4 can also be used as capable visible light photocatalyst for degradation of dangerous contaminants and for reduction of carcinogenic Cr(VI) into nontoxic Cr(III) from waste water.

Specific Hydrogen Spillover Pathways Generated on Graphene Oxide Enabling the Formation of Non-Equilibrium Alloy Nanoparticles.

The phenomenon of hydrogen spillover is investigated as a means of realizing a hydrogen-based society for over half a century. Herein, a graphene oxide having a precisely tuned architecture via calcination in air to introduce ether groups onto basal planes along with carbon defects is reported. This material provides specific pathways for the spillover of atomic hydrogen and has practical applications with regard to the synthesis of non-equilibrium solid-solution alloy nanoparticles. A combination of experimental work and simulations confirmed that the presence of ether groups associated with carbon defects facilitated hydrogen spillover within the basal planes of this graphene oxide. This enhanced hydrogen spillover ability, in turn, enables the simultaneous reduction of Ru3+ and Ni2+ ions to form RuNi alloy nanoparticles under hydrogen reduction conditions. Energy dispersive X-ray and X-ray absorption near edge structure simulations establish that this strategy forms unique alloy nanoparticles each comprising a Ru core with a RuNi solid-solution shell having a hexagonal close-packed structure. These non-equilibrium RuNi alloy nanoparticles exhibit greater catalytic activity than monometallic Ru nanoparticles during the hydrolysis of ammonia borane.

Bimetallic Gold–Iron Oxide Nanoparticles as Carriers of Methotrexate: Perspective Tools for Biomedical Applications

Bimetallic nanoparticles (BMNPs) combine unique and synergistic properties of two metals, allowing new specific applications. In this study, bimetallic AuFe nanoparticles and their conjugates with methotrexate (MTX) were obtained with an environmentally safe method of metal-vapor synthesis. The composition and electronic structure of the particles were investigated with X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray (EDX) spectrum and X-ray absorption spectroscopy (XANES and EXAFS). The effects of BMNP-MTX conjugates on human primary cells and tumor cell lines were evaluated with neutral red uptake and MTT in vitro cytotoxicity assays. Bright-field microscopy analyses of tumor spheroid size and evaluations of tumor spheroid vitality based on SFDA AM staining were carried out. In vitro assays for an antibacterial activity evaluation of the generated samples were performed. The influence of BMNP-MTX on cytokine production with normal leukocytes was assessed using ELISA. X-ray analyses of the samples demonstrated that gold was in the ground state Au0 as well as Au+ and Au3+ states are present in small quantities, whereas iron existed as a mixture of non-histometric oxides with states close to Fe2+ and Fe3+. The modification of the AuFe system with MTX is accompanied by a threefold increase in the relative proportion of the Au+ state. BMNP-MTX conjugates demonstrated significant antitumor activity compared to the drug alone, which proves the ability of the generated nanoconjugates to improve the effectiveness of MTX therapy. This was confirmed by a marked reduction in the size and vitality of AuFe-MTX-treated 3D tumor spheroids. In addition to their selective antitumor activity, AuFe-MTX exhibited moderate antibacterial activity and induced sample-specific cytokine production with normal human leukocytes—which points to an immunostimulatory potential. The present findings indicate important and diverse biological properties of BMNP-MTX conjugates and thus highlight perspectives for their biomedical applications and new immune-specific abilities.

Tweaking and collating the structural, optical and magnetic properties of auto combusted lanthanum ferrites - study on effect of precursor concentration

A novel sol-gel auto-combustion technique is utilized to prepare nano-sized, perovskite-structured LaFeO3 powders. The nanoparticles were synthesized for three distinct precursor concentrations (0.5, 1 and 1.5 M) maintaining pH, annealing temperature and time. The synthesized nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, high-resolution scanning electron microscopy (HRSEM), high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray absorption spectroscopy (EDAX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) study and vibrating sample magnetometer (VSM). XRD revealed that all the prepared samples have shown an orthorhombic phase with space group Pnma. DRS suggested a marginal increase in bandgap and the average band gap was found to be 2.2 eV VSM analysis has shown that all the prepared samples exhibit weak ferromagnetic behaviour due to uncompensated canted spins. All the studies performed revealed a significant modification of structural, optical and magnetic properties with the variation of precursor concentration.

Accumulative Delocalized Mo 4d Electrons to Bound the Volume Expansion and Accelerate Kinetics in Mo6S8 Cathode for High-Performance Aqueous Cu2+ Storage.

Electronic structure defines the conductivity and ion absorption characteristics of a functional electrode, significantly affecting the charge transfer capability in batteries, while it is rarely thought to be involved in mesoscopic volume and diffusion kinetics of the host lattice for promoting ion storage. Here, we first correlate the evolution in electronic structure of the Mo6S8 cathode with the ability to bound volume expansion and accelerate diffusion kinetics for high-performance aqueous Cu2+ storage. Operando synchrotron energy-dispersive X-ray absorption spectroscopy reveals that accumulative delocalized Mo 4d electrons enhance the Mo-Mo interaction with distinctly contracting and uniformizing Mo6 clusters during the reduction of Mo6S8, which potently restrain lattice expansion and release space to promote Cu2+ diffusion kinetics. Operando synchrotron X-ray diffraction and comprehensive characterizations further validate the structural and electrochemical properties induced by the Cu2+ intercalation electronic structure, endowing the Mo6S8 cathode a high specific capacity with small volume expansion, fast ions diffusion, and long-term cycling stability.

Purity and properties of spherical shaped Co3O4 nanocrystals prepared by a polyol route using a domestic microwave oven

Obtaining spherical shaped Co3O4 nanocrystals/nanoparticles (considered to be a very promising functional material) at low-cost with chemical purity, reduced crystallite size and useful physicochemical properties has been considered to be challenging. The present work (an attempt in this direction) involves the preparation of spherical shaped Co3O4 nanocrystals from cobalt acetate (dissolved in ethylene glycol) by a polyol synthesis route using a domestic microwave oven along with calcination at a suitable temperature (100/200/300/400 °C used to understand the phase evolution). X-ray diffraction (XRD, including Rietveld), infrared spectral, Raman spectral, energy dispersive X-ray absorption spectral and electron microscopic (SEM/TEM, including SAED) analyses have shown good crystallinity, chemical phase purity, spherical shape, reduced crystallite/particle size and narrow size distribution for the Co3O4 nanocrystal sample calcined at 400 °C. UV-Vis-NIR spectral analysis has shown the existence of multiple bandgap energies (1.51–1.98, 2.44–2.61 and 2.81–3.43 eV). Magnetic measurements have confirmed the antiferromagnetic nature possessing considerable magnetization below and above Neel temperature (TN), which indicates the presence of weak ferromagnetic ordering. The crystallite/particle sizes obtained for the sample calcined at 400 °C through XRD analysis, TEM analysis and using TN value (37.3 K) are 32.0, 33.6 and 31.3 nm, respectively. The method of preparation used is highly yielding, low-cost and more advantageous than many other methods used in the past.

In-vivo anticoccidial efficacy of green synthesized iron-oxide nanoparticles using Ficus racemosa Linn leaf extract. (Moraceae) against Emeria tenella infection in broiler chicks

Coccidiosis is an acute gastrointestinal parasitic disease and causes approximately $2.80 to $3.27 per m2 loss in a broiler farm of a 33-day-old flock. In this study, iron oxide nanoparticles (IONPs) were green synthesized using the aqueous leaf extract of Ficus racemosa as a reducing and capping agent to reduce the emerging resistance in coccidia spores against conventional treatments and boost the immune level in broilers. These IONPs were evaluated for their impacts on the growth performance, biochemistry, blood profile, and histology in the coccidiodized broiler chicken with Emeria tenella under in vivo conditions. The characteristics and stability of particles were obtained using UV-Vis spectroscopy, Fourier transforms infrared (FTIR), X-Ray diffraction (XRD), energy dispersive X-ray absorption (EDX), scanning electron microscopy (SEM), zeta potential and zeta size. The results indicated that IONPs at the moderate dose of 15 mg/kg (p = 0.001) reduced the coccidial impacts by eliminating oocyst shedding per gram feces (up to 91%) and reducing clinical symptoms (lesions (LS = 0), bloody diarrhea (No), and mortality (0%) in chicken at day 10 of treatment as compared to the negative control group-B (infected & non-treated). A dose-dependent and time-dependent trend were observed during treatments (10, 15, and 20 mg/kg) of 1–3 weeks using IONPs against the coccidial impacts on the growth parameters (body weight gain, mean feed consumption, feed conversion ratio) and biochemistry (plasma glucose, total protein, uric acid, ALT, AST, and ALP) in chickens. Additionally, F. racemosa IONPs at a dose of 15 and 20 mg/kg significantly recovered the parasitized and highly damaged hepatocytes, liver tissues, and ceca tissues after 1–3 weeks of treatment in broiler chickens. Overall, the 15 mg/kg concentration of IONPs exhibited fast recovery and growth enhancement in coccidiodized broilers. Therefore, the 15 mg/kg dose of green synthesized IONPs using leaf extract of F. racemosa could be a potential and safe anticoccidial agent with targeted implications in the poultry industry.

Ultrastable Cu2+ Intercalation Chemistry Based on a Niobium Sulfide Nanosheet Cathode for Advanced Aqueous Storage Devices

Exploring stable and durable cathodes for cost-effective reversible aqueous batteries is highly desirable for grid-scale energy storage applications, but significant challenges remain. Herein, we disclosed an ultrastable Cu2+ intercalation chemistry in mass-produced exfoliated NbS2 nanosheets to build ultralong lifespan aqueous batteries with cost advantages. Anisotropic interplanar expansion of NbS2 lattices balanced dynamic Cu2+ incorporation and the highly reversible redox reaction of Nb4+/Nb(4-δ)+ couple were illuminated by operando synchrotron X-ray diffraction and energy dispersive X-ray absorption spectroscopy, affording an extraordinary capacity of approximately 317 mAh g-1 at 1 A g-1 and a good stability of 92.2% capacity retention after 40000 cycles at 10 A g-1. Impressively, a budget NbS2||Fe hybrid ion cell involving an aqueous electrolyte/Fe-metal anode is established and provides a reliable energy supply of 225.4 Wh kg-1 at 750 W kg-1, providing insights for building advanced aqueous battery systems for large-scale applications.

Determining the proton diffusion coefficient in highly hydrated iridium oxide films by energy dispersive X-ray absorption spectroscopy

Charge transfer reactions in electrodeposited iridium oxide films (EIROF) are investigated by means of operando energy dispersive X-ray absorption spectroscopy (EDXAS), where oxidation and reduction conditions are selected to drive the Ir(III)/Ir(IV) and Ir(IV)/Ir(V) reactions in acidic solutions. The Ir(III)/Ir(IV) couple is related to a well-known electrochromic phenomenon, while the Ir(IV)/Ir(V) couple might play an important role in the catalysis of the oxygen evolution reactions (OER). In the experiments, current intensity and time-resolved X-ray absorption spectroscopy (XAS) are simultaneously recorded upon application of appropriate potential steps, leading to the independent determination of both the relevant reaction rates and the rate-determining steps. This is allowed by the fast acquisition time (∼10−2 s) at the ESRF Energy Dispersive XAS (EDXAS) ID24 beam-line, in combination with the highly hydrated amorphous iridium oxide electrode material, which in turn allows to maximize the fraction of Ir sites participating in the electrochemical processes. If the experimental conditions exclude the possibility of having either oxygen evolution (or reduction), the Degree of Reaction (DoR), determined by both electrochemistry and XAS, exhibits exponential time dependence, clearly pointing to diffusion-controlled processes. Vice versa, under concomitant OER + oxidation of iridium centers or ORR + iridium reduction, the electrochemical and XAS DoRs highlight different phenomena, providing fully complementary information of the ongoing electrode reactions. In all cases, data elaboration allows to determine the diffusion coefficient of H+ ions within the catalyst layer, that is compared and confirmed by data obtained by electrochemical impedance spectroscopy (EIS). The high values of D obtained for EIROF is compared to values obtained on other IrO2 materials can help in explaining the relevant high electrocatalytic activity.

Evolution of the perovskite phase in UO2-based samples under conditions representative of a severe nuclear accident by XANES

To understand the fission products behaviour during a Nuclear Severe Accident (NSA), simulated high burnup UO2 fuels produced by sintering at high temperature (SIMFUEL) were submitted to thermal treatments in conditions representative of the beginning of a Pressurized Water Reactor (PWR) severe accident. The samples made of UO2 doped with eleven fission products (FP) surrogates were thus thermally treated from 400 ​°C up to 1000 ​°C at different oxygen potentials (up to −290 ​kJ ​mol(O2)−1 at 1000 ​°C). The samples were characterized before and after the heat treatments by Secondary Electron Microscopy coupled with Energy Dispersive X-ray Spectroscopy (SEM-EDX) and X-ray Absorption Spectroscopy (XAS) at the MARS beamline, SOLEIL Synchrotron and at the FAME-UHD beamline, ESRF. Initially the SIMFUEL is constituted of a UO2 matrix, a metallic phase composed of Mo, Pd, Ru, Rh and Tc, and an oxide phase with perovskite structure depicted as (Ba, Sr)(Zr, U, RE)O3 where RE stands for Rare Earths. Around 1000 ​°C, it was found that Mo, initially contained in the metallic inclusions, oxidizes into MoO2. In the same conditions, a part of the oxidized Mo interacts with the perovskite phase containing Ba to form BaMoO4. These results will be useful to validate the theoretical models used in calculation codes and to assess thermodynamic databases, which are one of the main sources of errors when calculating a NSA sequence involving molten fuel.

Reduced Graphene Oxide–Metal Oxide Nanocomposites (ZrO2 and Y2O3): Fabrication and Characterization for the Photocatalytic Degradation of Picric Acid

Herein, reduced graphene-oxide-supported ZrO2 and Y2O3 (rGO-ZrO2 and rGO-Y2O3) nanocomposites were synthesized by hydrothermal method and used as the catalysts for photodegradation of picric acid. The structural and morphological properties of the synthesized samples were characterized by using an X-ray diffractometer (XRD), scanning electron microscope (SEM) with energy dispersive absorption X-ray spectroscopy (EDAX), UV-Vis spectrophotometer, Raman spectrophotometer and Fourier transformation infrared spectrophotometer (FT-IR) techniques. In this work, the wide band gap of the ZrO2 and Y2O3 was successfully reduced by addition of the reduced graphene oxide (rGO) to absorb visible light for photocatalytic application. The performance of as synthesized rGO-ZrO2 and rGO-Y2O3 nanocomposites in the photocatalytic degradation of picric acid were evaluated under UV light irradiation. The photodegradation study using picric acid was analyzed with different energy light sources UV (254, 365 and 395 nm), visible light and sunlight at different pH conditions (pH = 3, 7 and 10). The photocatalytic activity of rGO-ZrO2 and rGO-Y2O3 nanocomposites showed excellent photocatalytic activity under optimum identical conditions with mild variations in pH 3. Compared to rGO-Y2O3, the rGO-ZrO2 nanocomposite showed a better action, with a degradation percentage rate of 100, 99.3, 99.9, 100 and 100% for light conditions of UV-252, 365, 395, visible and sunlight, respectively. The excellent degradation efficiency is attributed to factors such as oxygen-deficient metal oxide phase, high surface area and creation of a greater number of hydroxyl groups.

In-situ X-ray studies of high-entropy layered oxide cathode for sodium-ion batteries

High-entropy oxides (HEOs) are promising electrode materials for sodium-ion batteries (SIBs) owing to their remarkable electrochemical properties and excellent cycling stability. A high-entropy O3-type layer-structured NaCu 0.1 Ni 0.3 Fe 0.2 Mn 0.2 Ti 0.2 O 2 (NCNFMT) was synthesized using the Pechini method, as a new cathode material for SIBs. Herein, density functional theory calculations were used to understand the formation energy of NCNMFT, proving its synthesizability. Battery testing revealed a reversible capacity of 130 mAh g −1 , with a capacity retention of up to 87% after 100 cycles at 0.1C, and excellent long-term cycling stability (approximately 71% after 500 cycles at 0.5C). The prepared material also exhibited an outstanding Coulombic efficiency of 98% and a high energy efficiency of 95%. Furthermore, the high entropy effect was investigated using energy dispersive spectroscopy and X-ray absorption fine structure to prove that the material contains a single phase with well-distributed metal ions. The operando synchrotron X-ray diffraction demonstrated that the phase transition was delayed until the extraction of 0.32 sodium ion from NCNFMT, which indicates the stabilization of the O3-phase induced by the high entropy effect. Furthermore, the quasi-solid-state NCNFMT||polyethylene oxide-Na 3.2 Ca 0.1 Zr 1.9 Si 2 PO 12 ||Na cells exhibited excellent performance with a high discharge capacity of 112 mAh g −1 and retention of 78% after 100 cycles. The above results demonstrate the advantages of HEOs as potential cathode materials for SIBs.

Ag nanoparticles synthesized by Datura metel L. Leaf extract and their charge density distribution, electrochemical and biological performance

The present study investigates the electrochemical performance; charge density distribution, antimicrobial and antifungal activities of green synthesized silver nanoparticles (Ag NPs) using the leaf extract of Datura metel L. UV–vis absorption spectrum shows that highly stable, monodispersed Ag NPs formed at 418 nm. Particle size analysis with zeta potential values 117 nm, − 27.3 mV are implied that hydrodynamic size with negative surface charges. Fourier transforms infrared (FTIR) analysis identified amide functional groups in Datura metel L. responsible for the reduction and stabilization of nanoparticles. Scanning electron microscopy (SEM) analysis showed about the spherical morphology and Energy Dispersive Absorption X-ray (EDAX) spectrum displays the Ag peak at 3.1 KeV with encapsulation of organic trace elements. X-ray Photoelectron Spectroscopy (XPS) analysis exhibit’s Ag 3d, Ag 3p, and Ag 3s chemical state of Ag NPs and the X-ray Diffraction (XRD) pattern confirmed the crystalline nature at 38.1˚ with organometallic phases. The structure factors in the single unit cells are studied in about three, two, and one-dimensional profiles using the Rietveld refinement technique. The complex of atropine with the nanoparticle was modeled using the MOPS method. The formation of the complex is carried out due to the transfer of the electron density of Ag NPs to the atropine molecule, which consists of more electronegative atoms. A charge transfer complex in which the nanoparticle acquires a charge of +0.354 and the atropine – 0.354 is formed. The synthesized Ag NPs exhibited noticeable antimicrobial, antifungal activity with large–diameter inhibition zones against S. pyogenes (12.1 ± 0.66 mm), E. faecalis (11.8 ± 0.33 mm), K. pneumoniae (10.2 ± 0.44 mm), S. flexneri (10.3 ± 0.21 mm), C. albicans (11.3 ± 0.66 mm), and A. fumigatus (10.5 ± 0.33 mm). The green synthesized Ag NPs as prepared electrode exhibits specific capacitance of 825 F/g at the current density of 3 mA/g in 1 M KOH electrolyte solution and cyclic stability retained at about 88.35% even after 5000 cycles with the current density of 5 mA/g. The results showed their effective utilization of green synthesized Ag NPs in biological and electrochemical storage applications.

Bio-approach: preparation of RGO-AgNPs on cotton fabric and interface with sweat environment for antibacterial activity.

This study aims to develop a reduced graphene oxide (RGO)-silver nanoparticles (AgNPs) coating on the cotton fabric (CT) surface using photoreduction with a hydrothermal process and evaluate the antibacterial activity in a sweat environment. An ureolytic bacterium of Bacillus subtilis (HM475276) was used to generate ammonia from synthetic urine. RGO-AgNPs were synthesizedon the CT surface using a moderate dosage of 1% silver ammonium complex. The analytical study reveals that spherical-shaped AgNPs of 10-50nm size were uniformly anchored throughout the RGO sheet on the CT, further supported by X-ray photoelectron spectroscopic analysis (XPS). X-raypowder diffraction (XRD) and Energy-dispersive X-ray absorption spectroscopy (EDAX) elemental mapping confirmed Ag/AgCl formation on CT treated with sweat. The sustained release of Ag+ ions from the treated CT in the sweat solution was assessed by atomic absorption spectroscopy (AAS) and ranged from 2 to 8ppm, correlated with antibacterial activity. The agar diffusion and solution suspension method to demonstrate the combat bacterial species were greater on RGO-AgNPs-CT than sweat-treated CT due to the suppression of Ag+ ion release caused by the deposition of Ag/AgCl. Hence, sweat-treated RGO-AgNPs-CT proved to have higher inactivation activity (45min) than sweat-treated AgNPs-CT (60min) due to the RGO-Ag/AgCl serving photocatalyst influencing hydroxyl radical (OH·) formation under sunlight. The RGO-AgNPs-CT has confirmed that it retains antibacterial activity after passing the laundry durability test. Together, the results showed an opportunity for improved functional fabrics that are exceptional at combating bacterial pathogens and holding up well to laundry durability tests.

Zinc Oxide Nanoparticles (ZnO NPs), Biosynthesis, Characterization and Evaluation of Their Impact to Improve Shoot Growth and to Reduce Salt Toxicity on Salvia officinalis In Vitro Cultivated

Green synthesis of zinc oxide nanoparticles (ZnO NPs) using plant extracts have recently attracted considerable attention due to their environmental protection benefits and their easy and low cost of fabrication. In the current study, ZnO NPS were synthesized using the aqueous extract of Ochradenus arabicus as a capping and reducing agent. The obtained ZnO NPs were firstly characterized using ultraviolet visible (UV-Vis) spectroscopy, Fourier transform infrared (FTIR), transmission electron microscope (TEM), X-ray diffraction (XRD), energy dispersive X-ray absorption (EDX), zeta potential, and zeta size. All these techniques confirmed the characteristic features of the biogenic synthesized ZnO NPs. Then, ZnO NPs were evaluated for their effects on morphological, biochemical, and physiological parameters of Salvia officinalis cultured in Murashige and Skoog medium containing 0, 75, 100, and 150 mM of NaCl. The results showed that ZnO NPs at a dose of 10 mg/L significantly increased the shoot number, shoot fresh weight, and shoot dry weight of Salvia officinalis subjected or not to the salt stress. For the shoot length, a slight increase of 4.3% was recorded in the plant treated by 150 mM NaCl+10 mg/L ZnO NPs compared to the plant treated only with 150 mM of NaCl. On the other hand, without NaCl, the application of both concentrations 10 mg/L and 30 mg/L of ZnO NPs significantly improved the total chlorophyll content by 30.3% and 21.8%, respectively. Under 150 mM of NaCl, the addition of 10 mg/L of ZnO NPs enhanced the total chlorophyll by 1.5 times, whilst a slight decrease of total chlorophyll was recorded in the plants treated by 150 mM NaCl + 30 mg/L ZnO NPs. Additionally, ZnO NPs significantly enhance the proline accumulation and the antioxidative enzyme activities of catalase (CAT), superoxide dismutase (SOD), and glutathione reductase (GR) in plants under salinity. Our findings revealed that green synthesized ZnO NPs, especially at a dose of 10 mg/L, play a crucial role in growth enhancement and salt stress mitigation. Hence, this biosynthesized ZnO NPs at a concentration of 10 mg/L can be considered as effective nanofertilizers for the plants grown in salty areas.

Deoxydehydration of Biomass-Derived Polyols Over Silver-Modified Ceria-Supported Rhenium Catalyst with Molecular Hydrogen.

Olefin production from polyols via deoxydehydration (DODH) was carried out over Ag-modified CeO2 -supported heterogeneous Re catalysts with H2 as a reducing agent. Both high DODH activity and low hydrogenation ability for C=C bonds were observed in the reaction of erythritol, giving a 1,3-butadiene yield of up to 90 % under "solvent-free" conditions. This catalyst is applicable to other substrates such as methyl glycosides (methyl α-fucopyranoside: 91 % yield of DODH product; methyl β-ribofuranoside: 88 % yield), which were difficult to be converted to the DODH products over the DODH catalysts reported previously. ReOx -Ag/CeO2 was reused 3 times without a decrease of activity or selectivity after calcination as regeneration. Although the transmission electron microscopy energy-dispersive X-ray spectroscopy and X-ray absorption fine structure analyses showed that Re species were highly dispersed and Ag was present as metal particles with various sizes from well-dispersed species (<1 nm) to around 5 nm particles, the catalysts prepared from size-controlled Ag nanoparticles showed similar performance, indicating that the catalytic performance is insensitive to the Ag particle size.

SILAR Synthesized ZnO Thin Films

Zinc oxide (ZnO) thin films are synthesized by using modified successive ionic layer adsorption and reaction techniques (SILAR) on glass substrate at room temperature. These as deposited thin films are characterized for structural, compositional, surface morphology and optical characterizations using X-ray diffraction (XRD), energy dispersive X-ray absorption spectra analysis (EDAX), atomic force microscopy (AFM) and Uv-vis absorption spectroscopy. From XRD pattern; the low intensity peaks indicate that the films consist coarsely fine grains and/or amorphous in nature. The diffraction peaks observed at 2θ = 31.71 ̊, 36.27 ̊and 56.29 ̊ are attributed to (100), (101) and (110) planes having hexagonal phase while EDAX shows elemental traces for Zn and O. Surface morphology observed from the AFM corresponds granular shape evenly distributed over substrate surface.

Towards a dynamic compression facility at the ESRF.

Results of the 2018 commissioning and experimental campaigns of the new High Power Laser Facility on the Energy-dispersive X-ray Absorption Spectroscopy (ED-XAS) beamline ID24 at the ESRF are presented. The front-end of the future laser, delivering 15 J in 10 ns, was interfaced to the beamline. Laser-driven dynamic compression experiments were performed on iron oxides, iron alloys and bismuth probed by online time-resolved XAS.