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Sn3O4 are promising semiconductor materials due to their visible light absorption ability. In this work, a series of materials, such as SnO2, Sn3O4 and Sn3O4/SnO2 heterostructures, with different phase ratios were prepared using hydrothermal synthesis. The materials were characterized using X-ray diffraction (XRD), Raman and diffuse reflectance spectroscopy (DRS), high resolution transmission electron microscopy (HRTEM), nitrogen adsorption (BET). Flat-band potentials (EFB) of the samples were determined using the photocurrent onset potential (POP) method. It was shown that the potentials obtained with open circuit potential measurements versus illumination intensity (OCP) likely corresponded to the EFB of SnO2 nanoparticles in heterostructures due to interfacial electron transfer from the conducting band of Sn3O4 to that of SnO2. The photo-electrooxidation processes of a series of organic substrates were studied in the potential range of 0.6–1.4 V vs. RHE under irradiation with ultraviolet (λ = 370 nm) and visible (λ = 450 nm) light. The Sn3O4 sample showed high activity in the photo-electrooxidation of acetone and formic acid in visible light. The Sn3O4/SnO2 samples exhibited noticeable activity only in the oxidation of formic acid. The presence of the SnO2 phase in the Sn3O4/SnO2 samples increased the photocurrent values under ultraviolet illumination, but significantly reduced the oxidation efficiency in visible light. [ABSTRACT FROM AUTHOR]

We report an efficient method to synthesize undoped and K-doped rare cubic tungsten trioxide nanowires through the thermal evaporation of WO3 powder without a catalyst. The WO3 nanowires are reproducible and stable with a low-cost growth process. The thermal evaporation processing was conducted in a three-zone horizontal tube furnace over a temperature range of 550–850 °C, where multiple substrates were placed at different temperature zones. The processing parameters, including pressure, temperature, type of gas, and flow rate, were varied and studied in terms of their influence on the morphology, aspect ratio and density of the nanowires. The morphologies of the products were observed with scanning electron microscopy. High resolution transmission electron microscopy, X-ray photoelectron spectroscopy, and X-ray diffraction studies were conducted to further identify the chemical composition, crystal structure and growth direction of the nanostructures. Additionally, the growth mechanism has been proposed. Furthermore, we investigated the potassium doping effect on the physical properties of the nanostructures. Photoluminescence measurements show that there were shorter emission bands at 360 nm and 410 nm. Field emission measurements show that the doping effect significantly reduced the turn-on electric field and increased the enhancement factor. Furthermore, as compared with related previous research, the K-doped WO3 nanowires synthesized in this study exhibited excellent field emission properties, including a superior field enhancement factor and turn-on electric field. The study reveals the potential of WO3 nanowires in promising applications for sensors, field emitters and light-emitting diodes. [ABSTRACT FROM AUTHOR]

The growth of nanocrystals (NCs) from metal oxide-based substrates with exposed high-energy facets is of particular importance for many important applications, such as solar cells as photoanodes due to the high reactivity of these facets. The hydrothermal method remains a current trend for the synthesis of metal oxide nanostructures in general and titanium dioxide (TiO2) in particular since the calcination of the resulting powder after the completion of the hydrothermal method no longer requires a high temperature. This work aims to use a rapid hydrothermal method to synthesize numerous TiO2-NCs, namely, TiO2 nanosheets (TiO2-NSs), TiO2 nanorods (TiO2-NRs), and nanoparticles (TiO2-NPs). In these ideas, a simple non-aqueous one-pot solvothermal method was employed to prepare TiO2-NSs using tetrabutyl titanate Ti(OBu)4 as a precursor and hydrofluoric acid (HF) as a morphology control agent. Ti(OBu)4 alone was subjected to alcoholysis in ethanol, yielding only pure nanoparticles (TiO2-NPs). Subsequently, in this work, the hazardous chemical HF was replaced by sodium fluoride (NaF) as a means of controlling morphology to produce TiO2-NRs. The latter method was required for the growth of high purity brookite TiO2 NRs structure, the most difficult TiO2 polymorph to synthesize. The fabricated components are then morphologically evaluated using equipment, such as transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), electron diffraction (SAED), and X-ray diffraction (XRD). In the results, the TEM image of the developed NCs shows the presence of TiO2-NSs with an average side length of about 20–30 nm and a thickness of 5–7 nm. In addition, the image TEM shows TiO2-NRs with diameters between 10 and 20 nm and lengths between 80 and 100 nm, together with crystals of smaller size. The phase of the crystals is good, confirmed by XRD. The anatase structure, typical of TiO2-NS and TiO2-NPs, and the high-purity brookite-TiO2-NRs structure, were evident in the produced nanocrystals, according to XRD. SAED patterns confirm that the synthesis of high quality single crystalline TiO2-NSs and TiO2-NRs with the exposed {001} facets are the exposed facets, which have the upper and lower dominant facets, high reactivity, high surface energy, and high surface area. TiO2-NSs and TiO2-NRs could be grown, corresponding to about 80% and 85% of the {001} outer surface area in the nanocrystal, respectively. [ABSTRACT FROM AUTHOR]

Porous cerium oxide (ceria) nanoparticles were prepared with and without manganese (Mn) by using the flash combustion technique. Samples with different loadings (Ce/Mn ratio ranged from 100 to 10) were prepared by using a one-step process and water only as a solvent. Moreover, citric acid was utilized as a fuel in an aqueous medium, and the overall synthesis mixture was dried at 100 °C overnight and then calcinated at 550 °C for 3 h. The obtained final solid product was characterized by inductively coupled plasma (ICP), X-ray powder diffraction (XRD), diffuse reflectance ultraviolet-visible spectroscopy (DR-UV-Vis), and scanning electron microscopy (SEM), which was coupled with Energy Dispersive X-Ray Analysis (EDX), high resolution transmission electron microscopy (HR-TEM), and photoluminescence (PL) analysis. The characterization data showed that Mn ions were totally incorporated into the framework of ceria up to the applied loading. Under visible light illumination, the photocatalytic activity of the prepared samples was tested in the decolorization reaction of methyl green (MG) dye (wavelength greater than 425 nm). The results showed that increasing Mn content improved the photocatalytic activity of ceria. The sample with a Ce/Mn ratio of 10 performed 1.8 times better than bare porous ceria. Finally, the reusability of the best-performing sample was investigated in four consecutive runs without treatment, and slight deactivation was monitored after the fourth run. [ABSTRACT FROM AUTHOR]

Biodiesel has been recognized as an environmentally friendly, renewable alternative to fossil fuels. In this work, CaO/ZnCo2O4 nanocomposites were successfully synthesized via simple mechanochemical reaction between ZnCo2O4 and CaO powders by varying the CaO loading from 5 to 20 wt.%. The synthesized materials were found to be highly efficient heterogeneous catalysts for transesterification of tributyrin with methanol to produce biodiesel. The nanocomposite, which contained 20 wt.% CaO and 80 wt.% ZnCo2O4 (CaO/ZnCo2O4-20), exhibited superior and stable transesterification activity (98% conversion) under optimized reaction conditions (1:12 TBT to methanol molar ratio, 5 wt.% catalyst and 180 min. reaction time). The experimental results revealed that the reaction mechanism on the CaO/ZnCo2O4 composite followed pseudo first-order kinetics. The physicochemical characteristics of the synthesized nanocomposites were measured using X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM), Fourier-transformed infrared spectroscopy (FTIR), X-ray photoelectron spectrometer (XPS), N2-physisorption, and CO2- temperature-programmed desorption (CO2-TPD) techniques. The results indicated the existence of coalescence between the CaO and ZnCo2O4 particles, Additionally, the CaO/ZnCo2O4-20 catalyst was found to possess the greater number of highly basic sites and high porosity, which are the key factors affecting catalytic performance in transesterification reactions. [ABSTRACT FROM AUTHOR]

Photocatalysts based on g-C3N4 have been investigated in the CO2 reduction reaction under visible light irradiation (λ = 397, 427, 452 nm). Photocatalysts were prepared by melamine calcination at 500–600 °C with further platinum deposition (0.1–1.0 wt.%). The effect of the preparation conditions of g-C3N4 and the method of platinum deposition on the physicochemical properties and activity of photocatalysts was studied. The photocatalysts were investigated by X-ray photoelectron spectroscopy, X-ray absorption spectroscopy, X-ray diffraction, high resolution transmission electron microscopy, UV-Vis spectroscopy, and low temperature nitrogen adsorption techniques. It has been found that the efficiency of CO2 reduction is governed by the surface area of g-C3N4 and the presence of platinum in the metallic state, while the optimal content of platinum is 0.5 wt. %. The highest rate of CO2 reduction achieved over Pt/g-C3N4 photocatalyst is 13.2 µmol h−1 g−1 (397 nm), which exceeds the activity of pristine g-C3N4 by 7 times. The most active photocatalysts was prepared by calcining melamine in air at 600 °C, followed by modification with platinum (0.5 wt.%). [ABSTRACT FROM AUTHOR]

The interaction between IrO2 and TiO2 (anatase) in non-isothermal reduction conditions has been studied by the temperature programmed reduction technique. IrO2 clusters are of sizes between 0.5 and 0.9 nm as determined from High Resolution Transmission Electron Microscopy (HRTEM). Largely, two main regions for reduction were found and modeled at ca. 100 and 230 °C. The first region is attributed to the partial reduction of IrO2 clusters, while the second one is due to reduction of the formed crystalline (rutile IrO2), during TPR, to Ir metal. Two methods for calculating kinetic parameters were tested. First, by applying different ramping rates on a 3.5 wt.% IrO2/TiO2 using Kissinger's method. The apparent activation energy values for the first and second reduction regions were found to be ca. 35 and 100 kJ/mol, respectively. The second method was based on fitting different kinetic models for the experimental results in order to extract qualitative information on the nature of interaction during the reduction process. It was found that the first reduction is largely due to the amount of IrO2 (reactant concentration) while the second one involved phase boundary effect as well as nucleation. [ABSTRACT FROM AUTHOR]

Nitrogen-doped multi-walled carbon nanotubes (N-MWCNTs) are widely used for drug delivery. One of the main challenges is to clarify their interaction with hypoxia-inducible factor 1 alpha (HIF-1α), the lack of which leads to oncological and cardiovascular diseases. In the presented study, N-MWCNTs were synthesized by catalytic chemical vapor deposition and irradiated with argon ions. Their chemical state, local structure, interfaces, Stone–Wales defects, and doping with nitrogen were analyzed by high resolution transmission electron microscopy (HRTEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. Using experimental data, supercells of functionalized N-MWCNTs with an oxygen content of 2.7, 4 and 6 at. % in carboxyl groups were built by quantum chemical methods. Our analysis by the self-consistent charge density functional tight-binding (SCC DFTB) method shows that a key role in the functionalization of CNTs with carboxyl groups belongs to Stone–Wales defects. The results of research in the decoration of CNTs with HIF-1α demonstrate the possibility of wave-diffusion drug delivery. The nature of hybridization and relaxation determines the mechanism of oxygen regulation with HIF-1α molecules, namely, by OH-(OH–C) and OH-(O=C) chemical bonds. The concentration dependence of drug release in the diffusion mode suggests that the best pattern for drug delivery is provided by the tube with a carboxylic oxygen content of 6 at. %. [ABSTRACT FROM AUTHOR]

Membrane distillation (MD) is an emerging technology for water recovery from hypersaline wastewater. Membrane scaling and wetting are the drawbacks that prevent the widespread implementation of the MD process. In this study, coaxially electrospun polyvinylidene fluoride-co-hexafluoropropylene (PVDF-co-HFP) nanofibrous membranes were fabricated with re-entrant architecture and enhanced hydrophobicity/omniphobicity. The multiscale roughness was constructed by incorporating Al2O3 nanoparticles and 1H, 1H, 2H, 2H Perfluorodecyltriethoxysilane in the sheath solution. High resolution transmission electron microscopy (HR-TEM) could confirm the formation of the core-sheath nanofibrous membranes, which exhibited a water contact angle of ~142.5° and enhanced surface roughness. The membrane displayed a stable vapor flux of 12 L.m−2.h−1 (LMH) for a 7.0 wt.% NaCl feed solution and no loss in permeate quality or quantity. Long-term water recovery from 10.5 wt.% NaCl feed solution was determined to be 8–10 LMH with >99.9% NaCl rejection for up to 5 cycles of operation (60 h). The membranes exhibited excellent resistance to wetting even above the critical micelle concentration (CMC) for surfactants in the order sodium dodecyl sulphate (SDS) (16 mM) > cetyltrimethylammonium bromide (CTAB) (1.5 mM) > Tween 80 (0.10 mM). The presence of salts further deteriorated membrane performance for SDS (12 mM) and Tween-80 (0.05 mM). These coaxial electrospun nanofibrous membranes are robust and can be explored for long-term applications. [ABSTRACT FROM AUTHOR]

In the present work, Cu-doped ZnO nanostructures (Cu% = 0, 1, 5) have been prepared using microwave-assisted chemical route synthesis. The synthesized nanostructures were investigated through structural, morphological, optical, and magnetic characterizations. The results of the X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), and selective area electron diffraction (SAED) patterns confirmed that all of the samples exhibit the single-phase polycrystalline hexagonal crystal structure. The XRD results infer a decrease in the lattice parameters (a/c) by increasing the Cu% doping into ZnO. The field emission scanning electron microscopy (FE-SEM) and energy dispersive x-ray (EDX) spectroscopic measurements revealed the formation of nanostructures, showing the major elemental presence of Zn and O in the samples. The photoluminescence (PL) spectra exhibited photoemission in the UV and blue-green regions. With the increase in the Cu%, the photoemission in the UV region is reduced, while it is enhanced in the blue-green region. Raman spectra of the Cu-doped ZnO nanostructures displayed a blue shift of the E 2 High mode and an increase in the peak intensity of E1(LO), indicating the doping of Cu ion in the ZnO lattice. The dc magnetization measurements demonstrated the ferromagnetic behavior of all of the samples with an enhanced ferromagnetic character with increasing Cu%. [ABSTRACT FROM AUTHOR]

The adsorption-enhancing TiO2-SBA-15 photocatalyst has been synthesized by an in situ etching displacement method, which possesses unique regular hexagonal pores and large specific surface area. The as-prepared TiO2-SBA-15 can effectively adsorb and increase the concentration of pollutants in the photocatalyst and collision likelihood with the photogenerated radicals, thus improving the efficiency of photocatalytic organic degradation. The structure and morphology have been characterized by N2 adsorption isotherms, X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), and scanning electron microscopy (SEM). These characterizations confirm that TiF4 alcohol solution prefers to react with the internal surface of SBA-15 because of the Siphon effect. Fourier transform infrared (FTIR) spectra demonstrate that a Ti-O-Si bond formed after the reaction of TiF4 with SBA-15, which reveals a wonderful combination of TiO2 and SiO2 even at low temperatures. Through this function, the nanocomposite TiO2-SBA-15 could obviously improve the efficiency of photocatalytical removal of toluene in the gas phase. [ABSTRACT FROM AUTHOR]

The efficient use of renewable energy sources requires development of new electrocatalytic materials for electrochemical energy storage systems, particularly fuel cells. To increase durability of high temperature polymer electrolyte fuel cell (HT-PEMFC), Pt/carbon black based catalysts should be replaced by more durable ones, for example Pt/carbon nanofibers (CNF). Here, we report for the first time the quantitative ascorbic acid assisted deposition of Pt onto electrospun polyacrylonitrile-based CNF composite materials. The effect of their subsequent post-treatment at various temperatures (250 and 500 °C) and media (vacuum or argon-hydrogen mixture) on the Pt/C catalyst morphology is investigated. All obtained samples are thoroughly studied by high resolution electron microscopy, and Pt electrochemically active specific surface area was evaluated by cyclic voltammetry. [ABSTRACT FROM AUTHOR]

In this study, we synthesized polyacrylic acid (PAA)-Ca (Eu) nanoclusters as a luminescence sensor of phosphate ion by a complex method, and we aimed to achieve the quantitative detection of PO43− based on the sensitivity of the charge transfer band of Eu3+ to anionic ligand. The resulting PAA-Ca(Eu) nanoclusters showed a well-dispersed and a dot-like morphology, with an ultra-small diameter (the average size of 2.17 nm) under high resolution transmission electron microscopy(HRTEM) observation. A dynamic light scattering particle size analyzer (DLS) showed a hydrodynamic size of 2.39 nm. The (PAA)-Ca (Eu) nanoclusters as a luminescence sensor showed a significantly higher sensitivity for PO43− than other anions (CO32−, SiO32−, SO42−, SO32−, Br−, Cl−, F−). The luminescence intensity displayed a linear increase (y = 19.32x + 74.75, R2 > 0.999) in a PO43 concentration range (0–10 mM) with the concentration of PO43− increase, and the limit of detection was 0.023 mM. The results showed good recovery rates and low relative standard deviations. These (PAA)-Ca (Eu) nanoclusters are hopeful to become a luminescence sensor for quantitatively detecting PO43−. [ABSTRACT FROM AUTHOR]

Herein, we investigated the effect of the support modification (Sibunit carbon) with diazonium salts of Pd and Pd-Au catalysts on furfural hydrogenation under 5 bars of H2 and 50 °C. To this end, the surface of Sibunit (Cp) was modified with butyl (Cp-Butyl), carboxyl (Cp-COOH) and amino groups (Cp-NH2) using corresponding diazonium salts. The catalysts were synthesized by the sol immobilization method. The catalysts as well as the corresponding supports were characterized by Fourier transform infrared spectroscopy, N2 adsorption-desorption, inductively coupled plasma atomic emission spectroscopy, high resolution transmission electron microscopy, energy dispersive spectroscopy, X-ray diffraction, Hammet indicator method and X-ray photoelectron spectroscopy. The analysis of the results allowed us to determine the crucial influence of surface chemistry on the catalytic behavior of the studied catalysts, especially regarding selectivity. At the same time, the structural, textural, electronic and acid–base properties of the catalysts were practically unaffected. Thus, it can be assumed that the modification of Sibunit with various functional groups leads to changes in the hydrophobic/hydrophilic and/or electrostatic properties of the surface, which influenced the selectivity of the process. [ABSTRACT FROM AUTHOR]

The article presents the assessment of solutions and dried residues precipitated from solutions after the bioleaching process of Printed Circuit Boards (PCB) utilizing the Acidithiobacillus ferrooxidans. The obtained dried residues precipitated from bioleaching solution (leachate) and control solution were tested using morphology, phase, and chemical composition analysis, with particular emphasis on the assessment of crystalline and amorphous components. The analysis of the dried residues from leachate after bioleaching as well as those from the sterile control solution demonstrated a difference in the component oxidation—the leachate consisted of mainly amorphous spherical particles in diameter up to 200 nm, forming lacy aggregates. In the specimenform control solution larger particles (up to 500 nm) were observed with a hollow in the middle and crystalline outer part (probably Fe2O3, CuFeS2, and Cu2O). The X-ray diffraction phase analysis revealed that specimen obtained from leachate after bioleaching consisted mainly of an amorphous component and some content of Fe2O3 crystalline phase, while the dried residue from control solution showed more crystalline components. The share of the crystalline and amorphous components can be related to efficiency in dissolving metals during bioleaching. Obtained results of the investigation confirm the activity and participation of the A. ferrooxidans bacteria in the solubilization process of electro-waste components, with their visible degradation–acceleration of the reaction owing to a continuous regeneration of the leaching medium. The performed investigations allowed to characterize the specimen from leachate and showed that the application of complementary cross-check of the micro (SEM and S/TEM) and macro (ICP-OES and XRD) methods are of immense use for complete guidance assessment and obtained valuable data for the next stages of PCBs recycling. [ABSTRACT FROM AUTHOR]

In this manuscript, a novel dual-step selective epitaxy growth (SEG) of Ge was proposed to significantly decrease the defect density and to create fully strained relaxed Ge on a Si substrate. With the single-step SEG of Ge, the threading defect density (TDD) was successfully decreased from 2.9 × 107 cm−2 in a globally grown Ge layer to 3.2 × 105 cm−2 for a single-step SEG and to 2.84 × 105 cm−2 for the dual-step SEG of the Ge layer. This means that by introducing a single SEG step, the defect density could be reduced by two orders of magnitude, but this reduction could be further decreased by only 11.3% by introducing the second SEG step. The final root mean square (RMS) of the surface roughness was 0.64 nm. The strain has also been modulated along the cross-section of the sample. Tensile strain appears in the first global Ge layer, compressive strain in the single-step Ge layer and fully strain relaxation in the dual-step Ge layer. The material characterization was locally performed at different points by high resolution transmission electron microscopy, while it was globally performed by high resolution X-ray diffraction and photoluminescence. [ABSTRACT FROM AUTHOR]

Synchysite-(Ce) at Cinquevalli occurs as fine needles intergrown with quartz in quartz-dikes and in association with altered K-feldspar and oxidized chalcopyrite as major constituents. Synchysite-(Ce) [Ca1.00(Ce0.43La0.26Nd0.17Y0.07Pr0.04Sm0.02Gd0.01)Σ=1.00(CO3)2(F0.58(OH)0.42)], shows an overgrowth rim of bastnäsite-(Ce) [(Ce0.34La0.25Nd0.17Pb0.07C a0.06Y0.06Pr0.04S m0.02Gd0.01)Σ=1.00C O3(F0.75(OH)0.25)]. Unit cell refinement of synchysite (C2/c) and bastnäsite (P62c) led to a = 12.272(4), b = 7.100(2), c = 18.640(5) Å, β = 102.71(5)° , and a = 7.085(1), c = 9.746(2) Å, respectively. Polysomatic faults are sporadic, but polytypic disorder is widespread. High resolution transmission electron microscopy images taken along [100] or h130i show an apparent order and the related diffraction patterns are streak-free. Conversely, along [010] or h110i, a high density of stacking faults is observed and the related diffraction patterns show hhl rows with h , 3n affected by streaks. No ordered domain larger than a few unit cells was detected. The stacking sequence of (Ca,REE)-fluorcarbonates can be compared with subfamily-B mica polytypes (2M2, 2O and 6H), which are characterized by n·60° (n = odd) rotations. Subfamily-A polytypes (1M, 2M1 and 3T), characterized by n·60° (n = even) rotations, should not be possible. Synchysite, characterized by ±60° rotations, can be likened to the 2M2 polytype. [ABSTRACT FROM AUTHOR]

Partially occluded object detection (POOD) has been an important task for both civil and military applications that use high-resolution remote sensing images (HR-RSIs). This topic is very challenging due to the limited object evidence for detection. Recent partial configuration model (PCM) based methods deal with occlusion yet suffer from the problems of massive manual annotation, separate parameter learning, and low training and detection efficiency. To tackle this, a unified PCM framework (UniPCM) is proposed in this paper. The proposed UniPCM adopts a part sharing mechanism which directly shares the root and part filters of a deformable part-based model (DPM) among different partial configurations. It largely reduces the convolution overhead during both training and detection. In UniPCM, a novel DPM deformation deviation method is proposed for spatial interrelationship estimation of PCM, and a unified weights learning method is presented to simultaneously obtain the weights of elements within each partial configuration and the weights between partial configurations. Experiments on three HR-RSI datasets show that the proposed UniPCM method achieves a much higher training and detection efficiency for POOD compared with state-of-the-art PCM-based methods, while maintaining a comparable detection accuracy. UniPCM obtains a training speedup of maximal 10× and 2.5× for airplane and ship, and a detection speedup of maximal 7.2×, 4.1× and 2.5× on three test sets, respectively. [ABSTRACT FROM AUTHOR]

For every three people on the planet, there are approximately two Tonnes (Te) of plastic waste. We show that carbon recovery from polystyrene (PS) plastic is enhanced by the coaddition of solvents to grow carbon nanotubes (CNTs) by liquid injection chemical vapour deposition. Polystyrene was loaded up to 4 wt% in toluene and heated to 780 °C in the presence of a ferrocene catalyst and a hydrogen/argon carrier gas at a 1:19 ratio. High resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Raman spectroscopy were used to identify multiwalled carbon nanotubes (MWCNTs). The PS addition in the range from 0 to 4 wt% showed improved quality and CNT homogeneity; Raman "Graphitic/Defective" (G/D) values increased from 1.9 to 2.3; mean CNT diameters increased from 43.0 to 49.2 nm; and maximum CNT yield increased from 11.37% to 14.31%. Since both the CNT diameters and the percentage yield increased following the addition of polystyrene, we conclude that carbon from PS contributes to the carbon within the MWCNTs. The electrical contact resistance of acid-washed Bucky papers produced from each loading ranged from 2.2 to 4.4 Ohm, with no direct correlation to PS loading. Due to this narrow range, materials with different loadings were mixed to create the six wires of an Ethernet cable and tested using iPerf3; the cable achieved up- and down- link speeds of ~99.5 Mbps, i.e., comparable to Cu wire with the same dimensions (~99.5 Mbps). The lifecycle assessment (LCA) of CNT wire production was compared to copper wire production for a use case in a Boeing 747-400 over the lifespan of the aircraft. Due to their lightweight nature, the CNT wires decreased the CO2 footprint by 21 kTonnes (kTe) over the aircraft's lifespan. [ABSTRACT FROM AUTHOR]

The paper summarizes new information on the formation and functioning of Ni(acac)2-based multicomponent (Ziegler) systems for oligo- and polymerization of ethylene. It turns out that catalytically active sites formed in these systems are deposited on nickel-containing nanoparticles generated via the interaction of the starting components directly in the reaction system. It is shown that the activity, productivity, and composition of the target products depend on the water content in the initial solvent, all other things being equal. A model of nanosized nickel-containing particles formed during the interaction of Ni(acac)2 and diethylaluminum chloride or ethylaluminum sesquichloride is presented. [ABSTRACT FROM AUTHOR]

Ge-rich Ge–Sb–Te compounds are attractive materials for future phase change memories due to their greater crystallization temperature as it provides a wide range of applications. Herein, we report the self-assembled Ge-rich Ge–Sb–Te/Sb2Te3 core-shell nanowires grown by metal-organic chemical vapor deposition. The core Ge-rich Ge–Sb–Te nanowires were self-assembled through the vapor–liquid–solid mechanism, catalyzed by Au nanoparticles on Si (100) and SiO2/Si substrates; conformal overgrowth of the Sb2Te3 shell was subsequently performed at room temperature to realize the core-shell heterostructures. Both Ge-rich Ge–Sb–Te core and Ge-rich Ge–Sb–Te/Sb2Te3 core-shell nanowires were extensively characterized by means of scanning electron microscopy, high resolution transmission electron microscopy, X-ray diffraction, Raman microspectroscopy, and electron energy loss spectroscopy to analyze the surface morphology, crystalline structure, vibrational properties, and elemental composition. [ABSTRACT FROM AUTHOR]

In this work, the photocatalytic hydrogen evolution from ammonia borane under near-infrared laser irradiation at ambient temperature was demonstrated by using the novel core-shell upconversion-semiconductor hybrid nanostructures (NaGdF4:Yb3+/Er3+@NaGdF4@Cu2O). The particles were successfully synthesized in a final concentration of 10 mg/mL. The particles were characterized via high resolution transmission electron microscopy (HRTEM), photoluminescence, energy dispersive X-ray analysis (EDAX), and powder X-ray diffraction. The near-infrared-driven photocatalytic activities of such hybrid nanoparticles are remarkably higher than that with bare upconversion nanoparticles (UCNPs) under the same irradiation. The upconverted photoluminescence of UCNPs efficiently reabsorbed by Cu2O promotes the charge separation in the semiconducting shell, and facilitates the formation of photoinduced electrons and hydroxyl radicals generated via the reaction between H2O and holes. Both serve as reactive species on the dissociation of the weak B-N bond in an aqueous medium, to produce hydrogen under near-infrared excitation, resulting in enhanced photocatalytic activities. The photocatalyst of NaGdF4:Yb3+/Er3+@NaGdF4@Cu2O (UCNPs@Cu2O) suffered no loss of efficacy after several cycles. This work sheds light on the rational design of near-infrared-activated photocatalysts, and can be used as a proof-of-concept for on-board hydrogen generation from ammonia borane under near-infrared illumination, with the aim of green energy suppliers. [ABSTRACT FROM AUTHOR]

A novel nanomaterial Bacitracin-Ag Nanoclusters (Bacitracin-AgNCs) was formed to achieve a better antibacterial effect on Shigella flexneri which poses a serious threat to human health. In the current study, X-ray photoelectron spectrometer (XPS), Fourier transform infrared (FTIR), field-emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HR-TEM) and thermal gravimetric analysis (TGA) were used to characterize the properties of composited Bacitracin-AgNCs. Furthermore, the inhibitory effects of Bacitracin-AgNCs against S. flexneri were explored, and the inhibition mechanism was discussed in terms of its aspects of cell membrane ravage, ATPase activity decline and biofilm inhibition. The results reveal that the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of Bacitracin-AgNCs against S. flexneri were 0.03 mg/mL and 4 mg/mL. Bacitracin-AgNCs may cause irreversible impairment to cells and greatly change the cell morphology. The cell membrane integrity of S. flexneri was destroyed with changes in the characteristics of membrane permeability and intracellular substances leakage. Moreover, our study further proved that Bacitracin-AgNCs significantly inhibited the formation of S. flexneri biofilms and reduced the number of viable bacteria in biofilm. These findings provide a potential method for the exploitation of organic composite nanomaterials as a novel antimicrobial agent and its application in the food industry. [ABSTRACT FROM AUTHOR]

Power quality monitoring is a theme in vogue and accurate frequency measurement of the power line is a major issue. This problem is particularly relevant for power generating systems since the generated signal must comply with restrictive standards. The novelty of this work is the development of a smart sensor for real-time high-resolution frequency measurement in accordance with international standards for power quality monitoring. The proposed smart sensor utilizes commercially available current clamp, hall-effect sensor or resistor as primary sensor. The signal processing is carried out through the chirp z-transform. Simulations and experimental results show the efficiency of the proposed smart sensor. [ABSTRACT FROM AUTHOR]

In this paper, we present a blind image restoration algorithm to reconstruct a high resolution (HR) color image from multiple, low resolution (LR), degraded and noisy images captured by thin (< 1mm) TOMBO imaging systems. The proposed algorithm is an extension of our grayscale algorithm reported in [1] to the case of color images. In this color extension, each Point Spread Function (PSF) of each captured image is assumed to be different from one color component to another and from one imaging unit to the other. For the task of image restoration, we use all spectral information in each captured image to restore each output pixel in the reconstructed HR image, i.e., we use the most efficient global category of point operations. First, the composite RGB color components of each captured image are extracted. A blind estimation technique is then applied to estimate the spectra of each color component and its associated blurring PSF. The estimation process is formed in a way that minimizes significantly the interchannel cross-correlations and additive noise. The estimated PSFs together with advanced interpolation techniques are then combined to compensate for blur and reconstruct a HR color image of the original scene. Finally, a histogram normalization process adjusts the balance between image color components, brightness and contrast. Simulated and experimental results reveal that the proposed algorithm is capable of restoring HR color images from degraded, LR and noisy observations even at low Signal-to-Noise Energy ratios (SNERs). The proposed algorithm uses FFT and only two fundamental image restoration constraints, making it suitable for silicon integration with the TOMBO imager. [ABSTRACT FROM AUTHOR]

This paper presents an optical measuring system based on low cost, high resolution digital cameras. Once the cameras are synchronised, the portable and adjustable system can be used to observe living beings, bodies in motion, or deformations of very different sizes. Each of the cameras has been modelled individually and studied with regard to the photogrammetric potential of the system. We have investigated the photogrammetric precision obtained from the crossing of rays, the repeatability of results, and the accuracy of the coordinates obtained. Systematic and random errors are identified in validity assessment of the definition of the precision of the system from crossing of rays or from marking residuals in images. The results have clearly demonstrated the capability of a low-cost multiple-camera system to measure with sub-millimetre precision. [ABSTRACT FROM AUTHOR]

The matrix assisted pulsed laser evaporation (MAPLE) technique has been used for the deposition of metal dioxide (TiO2, SnO2) nanoparticle thin films for gas sensor applications. For this purpose, colloidal metal dioxide nanoparticles were diluted in volatile solvents, the solution was frozen at the liquid nitrogen temperature and irradiated with a pulsed excimer laser. The dioxide nanoparticles were deposited on Si and Al2O3 substrates. A rather uniform distribution of TiO2 nanoparticles with an average size of about 10 nm and of SnO2 nanoparticles with an average size of about 3 nm was obtained, as demonstrated by high resolution scanning electron microscopy (SEM-FEG) inspections. Gas-sensing devices based on the resistive transduction mechanism were fabricated by depositing the nanoparticle thin films onto suitable rough alumina substrates equipped with interdigitated electrical contacts and heating elements. Electrical characterization measurements were carried out in controlled environment. The results of the gas-sensing tests towards low concentrations of ethanol and acetone vapors are reported. Typical gas sensor parameters (gas responses, response/recovery time, sensitivity, and low detection limit) towards ethanol and acetone are presented. [ABSTRACT FROM AUTHOR]

A small-displacement sensor based on total-internal reflection theory and surface plasmon resonance technology is proposed for use in heterodyne interferometry. A small displacement can be obtained simply by measuring the variation in phase difference between s- and p-polarization states with the small-displacement sensor. The theoretical displacement resolution of the small-displacement sensor can reach 0.45 nm. The sensor has some additional advantages, e.g., a simple optical setup, high resolution, high sensitivity and rapid measurement. Its feasibility is also demonstrated. [ABSTRACT FROM AUTHOR]

This work investigates the degradation of the azo dye solochrome dark blue (SDB) by measurement of the photocatalytic, sonocatalytic and sonophotocatalytic activities, under low ultrasonic frequency (40 kHz) and UV-C (254 nm) light, using Mn-doped ZnS semiconductor quantum dots (Mn2+:ZnS Qds) as catalysts, prepared by a simple chemical precipitation procedure. In order to study the different morphological and optical crystal properties, various characterization techniques were used, such as high resolution transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray analysis, X-ray diffraction, N2 adsorption-desorption at −196 °C and ultraviolet-visible spectroscopy. The average particle size of the semiconductor Qds was in the range of 3–4 nm. The optimal parameters affecting dye degradation, such as the catalyst loading, solution pH, time of irradiation, initial concentration of dye, dopant concentration, ultrasonic power and frequency effect were evaluated. The synthesized catalytic material exhibited a high activity for sonophotocatalytic degradation of SDB (89%), larger than that observed for sonocatalysis (69.7%) or photocatalysis (55.2%) alone, which was due to the improved electron-holes separation, formation of more reactive radicals and enhancement of the active surface area. Qds showed good stability and reusability after five repeated cycles. Finally, the degradation products were identified by liquid chromatography-mass spectrometry (LC-MS). [ABSTRACT FROM AUTHOR]

In this work, we report the same trends for the contact potential difference measured by Kelvin probe force microscopy and the effective carrier lifetime on crystalline silicon (c-Si) wafers passivated by AlOx layers of different thicknesses and submitted to annealing under various conditions. The changes in contact potential difference values and in the effective carrier lifetimes of the wafers are discussed in view of structural changes of the c-Si/SiO2/AlOx interface thanks to high resolution transmission electron microscopy. Indeed, we observed the presence of a crystalline silicon oxide interfacial layer in as-deposited (200 °C) AlOx, and a phase transformation from crystalline to amorphous silicon oxide when they were annealed in vacuum at 300 °C. [ABSTRACT FROM AUTHOR]

Several aspects such as the growth relation between the layers of the GaN/AlN/SiC heterostructure, the consistency of the interfaces, and elemental diffusion are achieved by High Resolution Transmission Electron Microscopy (HR-TEM). In addition, the dislocation densities together with the defect correlation lengths are investigated via High-Resolution X-ray Diffraction (HR-XRD) and the characteristic positron diffusion length is achieved by Doppler Broadening Spectroscopy (DBS). Moreover, a comparative analysis with our previous work (i.e., GaN/AlN/Si and GaN/AlN/Al2O3) has been carried out. Within the epitaxial GaN layer defined by the relationship F 4 ¯ 3 m (111) 3C-SiC || P 63 m c (0002) AlN || P 63 m c (0002) GaN, the total dislocation density has been assessed as being 1.47 × 1010 cm−2. Compared with previously investigated heterostructures (on Si and Al2O3 substrates), the obtained dislocation correlation lengths (Le = 171 nm and Ls =288 nm) and the mean distance between two dislocations (rd = 82 nm) are higher. This reveals an improved crystal quality of the GaN with SiC as a growth template. In addition, the DBS measurements upheld the aforementioned results with a higher effective positron diffusion length L eff GaN 2 = 75 ± 20 nm for the GaN layer. [ABSTRACT FROM AUTHOR]

In this investigation, we showed that high salinity promoted by hydrothermal inputs, reducing conditions of sediments with high content in organic matter, and the occurrence of an appropriate clay mineral precursor provide a suitable framework for low-temperature illitization processes. We studied the sedimentary illitization process that occurs in carbonaceous sediments from a lake with saline waters (Sochagota Lake, Colombia) located at a tropical latitude. Water isotopic composition suggests that high salinity was produced by hydrothermal contribution. Materials accumulated in the Sochagota Lake's southern entrance are organic matter-poor sediments that contain detrital kaolinite and quartz. On the other hand, materials formed at the central segment and near the lake exit (north portion) are enriched in organic matter and characterized by the crystallization of Fe-sulfides. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), and energy dispersive X-ray spectrometry (EDX) data allowed for the identification of illite and illite-dioctahedral vermiculite mixed layers (I-DV), which are absent in the southern sediments. High humidity and temperate climate caused the formation of small-sized metastable intermediates of I-DV particles by the weathering of the source rocks in the Sochagota Lake Basin. These particles were deposited in the low-energy lake environments (middle and north part). The interaction of these sediments enriched in organic matter with the saline waters of the lake enriched in hydrothermal K caused a reducing environment that favored Fe mobilization processes and its incorporation to I-DV mixed layers that acted as mineral precursor for fast low temperature illitization, revealing that in geothermal areas clays in lakes favor a hydrothermal K uptake. [ABSTRACT FROM AUTHOR]

The microstructural evolution of dilute Al–Ag alloys in its early aging stage and at low temperatures ranging from 15 K to 300 K was studied by the combined use of Positron annihilation lifetime spectroscopy (PALS), high resolution transmission electron microscopy (HRTEM), and positron annihilation Coincidence Doppler broadening (CDB) techniques. It is shown that at low temperatures below 200 K, an Ag–vacancy complex is formed in the quenched alloy, and above 200 K, it decomposes into Ag clusters and monovacancies. Experimental and calculation results indicate that Ag clusters in Al–Ag alloys can act as shallow trapping sites, and the positron trapping rate is considerably enhanced by a decreasing measurement temperature. [ABSTRACT FROM AUTHOR]

Controllable growth of wafer-scale in-plane nanowires (NWs) is a prerequisite for achieving addressable and scalable NW-based quantum devices. Here, by introducing molecular beam epitaxy on patterned Si structures, we demonstrate the wafer-scale epitaxial growth of site-controlled in-plane Si, SiGe, and Ge/Si core/shell NW arrays on Si (001) substrate. The epitaxially grown Si, SiGe, and Ge/Si core/shell NW are highly homogeneous with well-defined facets. Suspended Si NWs with four {111} facets and a side width of about 25 nm are observed. Characterizations including high resolution transmission electron microscopy (HRTEM) confirm the high quality of these epitaxial NWs. [ABSTRACT FROM AUTHOR]

The effects of the wet milling rotating speed on the number of graphene layers and graphene quality, and the conversion efficiency of graphite exfoliate to graphene, were investigated by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). The results show that the number of few-layer graphene nanometer sheets (GNSs) (≤10 layers) gradually increases with the increase of rotational speed in the range of 160–240 rpm. The proportion of GNSs with 0–10 layers reaches more than 80% as the rotational speed is increased to 280 rpm. GNS defect types in the composite materials are marginal defects with minimal influence and almost no oxidation. In the range of 160–280 rpm, the intensity of graphite peak decreases and the conversion efficiency of graphene increases with the increase of rotational speed. This is the same as the experimental result obtained by HRTEM. [ABSTRACT FROM AUTHOR]

Oxidation of 5-hydroxymethylfurfural (HMF), a major feedstock derived from waste/fresh biomass, into 2,5-furandicarboxylic acid (FDCA) is an important transformation for the production of biodegradable plastics. Herein, we investigated the effect of the support (unmodified and modified titania, commercial alumina, and untreated and treated Sibunit carbon) of mono- and bimetallic catalysts based on noble metals (Ag, Au, Pd) on selective HMF oxidation with molecular oxygen to FDCA under mild and basic reaction conditions. The higher selectivity to FDCA was obtained when metals were supported on Sibunit carbon (Cp). The order of noble metal in terms of catalyst selectivity was: Ag < Au < Pd < PdAu. Finally, FDCA production on the most efficient PdAu NPs catalysts supported on Sibunit depended on the treatment applied to this carbon support in the order: PdAu/Cp < PdAu/Cp-HNO3 < PdAu/Cp-NH4OH. These bimetallic catalysts were characterized by nitrogen adsorption-desorption, inductively coupled plasma atomic emission spectroscopy, high resolution transmission electron microscopy, energy dispersive spectroscopy, X-ray diffraction, Hammet indicator method and X-ray photoelectron spectroscopy. The functionalization of Sibunit surface by HNO3 and NH4OH led to a change in the contribution of the active states of Pd and Au due to promotion effect of N-doping and, as a consequence, to higher FDCA production. HMF oxidation catalyzed by bimetallic catalysts is a structure sensitive reaction. [ABSTRACT FROM AUTHOR]

CoFe2O4 prepared by sol-gel has been examined with respect to its catalytic performance for preferential CO oxidation in a H2-rich stream. In turn, the promoting effects of incorporation of Ce, Co, Cu, and Zr by impregnation on the surface of CoFe2O4 on the process are examined as well. The catalysts have been characterized by N2 adsorption, X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM), temperature programmed reduction (TPR), and X-ray photoelectron spectra (XPS), as well as diffuse reflectance infrared DRIFTS under reaction conditions with the aim of establishing structure/activity relationships for the mentioned catalyst/process. It is shown that while the presence of the various metals on CoFe2O4 hinders a low temperature CO oxidation process, it appreciably enhances the activity above 125 °C. This is basically attributed to the surface modifications, i.e. cobalt oxidation, induced in CoFe2O4 upon introduction of the metals. In turn, no methanation activity is observed in any case except for the copper-containing catalyst, in which achievement of reduced states of cobalt appears most favored. [ABSTRACT FROM AUTHOR]

Tailoring the shape of nanoscale materials enables obtaining morphology-controlled surfaces exhibiting specific interactions with reactants during catalytic reactions. The specifics of nanoparticle surfaces control the catalytic performance, i.e., activity and selectivity. In this study, shape-controlled Platinum (Pt) and Palladium (Pd) nanoparticles with distinct morphology were produced, i.e., cubes and cuboctahedra for Pt and spheres and polyhedra/multiple-twins for Pd, with (100), (111 + 100), curved/stepped and (111) facets, respectively. These particles with well-tuned surfaces were subsequently deposited on a Zirconium oxide (ZrO2) support. The morphological characteristics of the particles were determined by high resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD), while their adsorption properties were investigated by Fourier transform infrared spectroscopy (FTIR) of CO adsorbed at room temperature. The effect of the nanoparticle shape and surface structure on the catalytic performance in hydrodechlorination (HDCl) of trichloroethylene (TCE) was examined. The results show that nanoparticles with different surface orientations can be employed to affect selectivity, with polyhedral and multiply-twinned Pd exhibiting the best ethylene selectivity. [ABSTRACT FROM AUTHOR]

In this paper we compare the photocatalytic activity of two semiconductors based on ZnO: ZnO/CeO2 and ZnO/Yb2O3. The two samples were prepared via hydrothermal synthesis and fully characterized by X-ray diffraction technique, diffuse reflectance Ultra Violet- Visible spectroscopy (UV-Vis), high resolution transmission electron microscopy and finally with electron paramagnetic resonance spectroscopy. The prepared materials were also tested in their photocatalytic performances both through Electron Paramagnetic Resonance (EPR) analyzing the formation of charge carriers and with the abatement of a probe molecule like phenol, in presence and in absence of scavengers. [ABSTRACT FROM AUTHOR]

It has been reported that improving electrical conductivity and maintaining stable structure during discharge/charge process are challenge for Si to be used as an anode for lithium ion batteries (LIB). To address this problem, milkweed (MW) was carbonized to prepare hollow carbon microtubes (HCMT) derived from biomass as an anode template for LIB. In order to improve electrical conductivity, various materials such as chitosan (CTS), agarose, and polyvinylidene fluoride (PVDF) are used as carbon source (C1, C2, and C3) by carbonization. Carbon coated HCMT@Si composits, HCMT@Si@C1, HCMT@Si@C1@C2, and HCMT@Si@C1@C3, have been successfully synthesized. Changes in structure and crystallinity of HCMT@Si composites were characterized by using X-ray diffraction (XRD). Specific surface area for samples was calculated by using BET (Brunauer–Emmett–Teller). Also, pore size and particle size were obtained by particle and pore size analysis system. The surface morphology was evaluated using high resolution scanning electron microscopy (HR-SEM), Field Emission transmission electron microscopy (TEM). The thermal properties of HCMT@Si composites were analyzed by thermogravimetric analysis (TGA). Our research was performed to study the synthesis and electrochemical performance of Si composite with HCMT by the carbonization of natural micro hollow milkweed to form an inner space. After carbonization at 900 °C for 2 h in N2 flow, inner diameter of HCMT obtained was about 10 μm. The electrochemical tests indicate that HCMT@Si@C1@C3 exhibits discharge capacity of 932.18 mAh/g at 0.5 A/g after 100 cycles. [ABSTRACT FROM AUTHOR]

Starting from subsurface Zr0-doped "inverse" Pd and bulk-intermetallic Pd0Zr0 model catalyst precursors, we investigated the dry reforming reaction of methane (DRM) using synchrotron-based near ambient pressure in-situ X-ray photoelectron spectroscopy (NAP-XPS), in-situ X-ray diffraction and catalytic testing in an ultrahigh-vacuum-compatible recirculating batch reactor cell. Both intermetallic precursors develop a Pd0–ZrO2 phase boundary under realistic DRM conditions, whereby the oxidative segregation of ZrO2 from bulk intermetallic PdxZry leads to a highly active composite layer of carbide-modified Pd0 metal nanoparticles in contact with tetragonal ZrO2. This active state exhibits reaction rates exceeding those of a conventional supported Pd–ZrO2 reference catalyst and its high activity is unambiguously linked to the fast conversion of the highly reactive carbidic/dissolved C-species inside Pd0 toward CO at the Pd/ZrO2 phase boundary, which serves the role of providing efficient CO2 activation sites. In contrast, the near-surface intermetallic precursor decomposes toward ZrO2 islands at the surface of a quasi-infinite Pd0 metal bulk. Strongly delayed Pd carbide accumulation and thus carbon resegregation under reaction conditions leads to a much less active interfacial ZrO2–Pd0 state. [ABSTRACT FROM AUTHOR]

The present work involves the development of a novel method for the fabrication of zirconium nickel (Zr(x)Ni(y)) alloy used as a nanocatalyst to improve the hydrogen storage properties of the Mg/MgH2 system. The catalyst was fabricated through the high-pressure reactor and activated under hydrogen prior to being mechanically milled with the MgH2 for 5 h under argon. The microstructure characterisation of the samples was determined via SEM-EDX (scanning electron microscope analysis–energy dispersive X-ray spectroscopy), XRD (X-ray diffraction) and FE-HRTEM (field emission high resolution transmission electron microscopy), and the desorption characteristic of the nanocomposite (10 wt.% Zr(x)Ni(y)–MgH2) was determined via TPD (temperature-programmed desorption). The nanostructured MgH2 powder milled with 10 wt.% of the activated Zr(x)Ni(y) based nanocatalyst resulted in a faster hydrogen release—5.9 H2-wt.% at onset temperature 210 °C/peak temperature 232 °C. The observed significant improvement in the hydrogen desorption properties was likely to be the result of the impact of the highly dispersed catalyst on the surface of the Mg/MgH2 system, the reduction in particle size during the ball milling process and/or the formation of Mg0.996Zr0.004 phase during the milling process. [ABSTRACT FROM AUTHOR]

Discovery of a novel anticancer drug delivery agent is important to replace conventional cancer therapies which are often accompanied by undesired side effects. This study demonstrated the synthesis of superparamagnetic magnetite nanocomposites (Fe3O4-NCs) using a green method. Montmorillonite (MMT) was used as matrix support, while Fe3O4 nanoparticles (NPs) and carrageenan (CR) were used as filler and stabilizer, respectively. The combination of these materials resulted in a novel nanocomposite (MMT/CR/Fe3O4-NCs). A series of characterization experiments was conducted. The purity of MMT/CR/Fe3O4-NCs was confirmed by X-ray diffraction (XRD) analysis. High resolution transmission electron microscopy (HRTEM) analysis revealed the uniform and spherical shape of Fe3O4 NPs with an average particle size of 9.3 ± 1.2 nm. Vibrating sample magnetometer (VSM) analysis showed an Ms value of 2.16 emu/g with negligible coercivity which confirmed the superparamagnetic properties. Protocatechuic acid (PCA) was loaded onto the MMT/CR/Fe3O4-NCs and a drug release study showed that 15% and 92% of PCA was released at pH 7.4 and 4.8, respectively. Cytotoxicity assays showed that both MMT/CR/Fe3O4-NCs and MMT/CR/Fe3O4-PCA effectively killed HCT116 which is a colorectal cancer cell line. Dose-dependent inhibition was seen and the killing was enhanced two-fold by the PCA-loaded NCs (IC50–0.734 mg/mL) compared to the unloaded NCs (IC50–1.5 mg/mL). This study highlights the potential use of MMT/CR/Fe3O4-NCs as a biologically active pH-responsive drug delivery agent. Further investigations are warranted to delineate the mechanism of cell entry and cancer cell killing as well as to improve the therapeutic potential of MMT/CR/Fe3O4-NCs. [ABSTRACT FROM AUTHOR]

Multifunctional hybrid materials with applications in gas sensing or dye removal from wastewaters were obtained by incorporation into silica matrices of either Pt(II)-5,10,15,20-tetra-(4-allyloxy-phenyl)-porphyrin (PtTAOPP) or platinum nanoparticles (PtNPs) alone or accompanied by 5,10,15,20-tetra-(4-allyloxy-phenyl)-porphyrin (TAOPP). The tetraethylorthosilicate (TEOS)-based silica matrices were obtained by using the sol-gel method performed in two step acid-base catalysis. Optical, structural and morphological properties of the hybrid materials were determined and compared by UV-vis, fluorescence and FT-IR spectroscopy techniques, by atomic force microscopy (AFM) and high resolution transmission electron microscopy (HRTEM) and by Brunauer–Emmett–Teller (BET) analysis. PtTAOPP-silica hybrid was the most efficient material both for CO2 adsorption (0.025 mol/g) and for methylene blue adsorption (7.26 mg/g) from wastewaters. These results were expected due to both the ink-bottle mesopores having large necks that exist in this hybrid material and to the presence of the porphyrin moiety that facilitates chemical interactions with either CO2 gas or the dye molecule. Kinetic studies concerning the mechanism of dye adsorption demonstrated a second order kinetic model, thus it might be attributed to both physical and chemical processes. [ABSTRACT FROM AUTHOR]

Tungsten trioxide (WO3) is a photocatalyst that has gained interest amongst researchers because of its non-toxicity, narrow band gap and superior charge transport. Due to its fast charge recombination, modification is vital to counteract this limitation. In this paper, we report on the fabrication of Mn-doped WO3/SnS2 nanoparticles, which were synthesised with the aim of minimising the recombination rates of the photogenerated species. The nanomaterials were characterised using spectroscopic techniques (UV-Vis-diffuse reflectance spectroscopy (DRS), Raman, XRD, photoluminescence (PL) and electrochemical impedance spectroscopy (EIS)) together with microscopic techniques (FESEM-EDS and high resolution transmission electron microscopy selected area electron diffraction (HRTEM-SAED)) to confirm the successful formation of Mn-WO3/SnS2 nanoparticles. The Mn-doped WO3/SnS2 composite was a mixture of monoclinic and hexagonal phases, confirmed by XRD and Raman analysis. The Mn-WO3/SnS2 heterojunction showed enhanced optical properties compared to those of the un-doped WO3/SnS2 nanoparticles, which confirms the successful charge separation. The Brunauer–Emmett–Teller (BET) analysis indicated that the nanoparticles were mesoporous as they exhibited a Type IV isotherm. These nanomaterials appeared as a mixture of rectangular rods and sheet-like shapes with an increased surface area (77.14 m2/g) and pore volume (0.0641 cm3/g). The electrochemical measurements indicated a high current density (0.030 mA/cm2) and low charge transfer resistance (157.16 Ω) of the Mn-WO3/SnS2 heterojunction, which infers a high charge separation, also complemented by photoluminescence with low emission peak intensity. The Mott–Schottky (M-S) plot indicated a positive slope characteristic of an n–n heterojunction semiconductor, indicating that electrons are the major charge carriers. Thus, the efficiency of Mn-WO3/SnS2 heterojunction photocatalyst was monitored for the degradation of chlorpyrifos. The effects of pH (3–9), catalyst loading (0.1–2 g) and initial chlorpyrifos concentration (100 ppb–20 ppm) were studied. It was observed that the degradation was purely due to photocatalysis, as no loss of chlorpyrifos was observed within 30 min in the dark. Chlorpyrifos removal using Mn-WO3/SnS2 was performed at the optimum conditions of pH = 7, catalyst loading = 1 g and chlorpyrifos concentration = 1000 ppb in 90 min. The complete degradation of chlorpyrifos and its major degradation by-product 3,5,6-trichloropyridin-2-ol (TCP) was achieved. Kinetic studies deduced a second order reaction at 209 × 10−3 M−1s−1. [ABSTRACT FROM AUTHOR]

Bifunctional catalysts on the base of transition metal sulfides (CoMoS and NiWS) and platinum as noble metal were synthesized via wetness impregnation of freshly synthesized Al2O3-SAPO-11 composites, supported with favorable acidic properties. The physical-chemical properties of the prepared materials were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), low-temperature N2 adsorption and high resolution transmission electron microscopy (HR TEM) methods. Catalytic properties were studied in n-hexadecane isomerization using a fixed-bed flow reactor. The catalytic poisons tolerance of transition metal sulfides (TMS)- and Pt-catalysts has been studied for sulfur and nitrogen, with the amount of 10–100 ppm addition to feedstock. TMS-catalysts show good stability during sulfur-containing feedstock processing, whereas Pt-catalyst loses much of its isomerization activity. Nitrogen-containing compounds in the feedstock has a significant impact on the catalytic activity of both TMS and Pt-based catalysts. [ABSTRACT FROM AUTHOR]

To characterize the interfacial microstructure and interaction at a nanoscale has a significant meaning for the interface improvement of the nanocomposites. In this study, the interfacial microstructure and features of aligned multiwalled carbon nanotube (MWNT) and conjugated polymer polyimide (PI) with three molecular structures were investigated using small-angle X-ray scattering (SAXS), wide-angle X-ray diffraction (WAXD), and fluorescence emission spectroscopy. It was found that aligned MWNT/PI nanocomposites had a nonideal two-phase system with the interfaces belonging to long period stacking ordered structure. Attributed to the π–π stacking effect, MWNT/BTDA-MPD presented the most regular arrangement verified by fractal dimension. By adopting a one-dimension correlation function, each phase dimension in aligned MWNT/PI nanocomposites was calculated and verified by high resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD). The π–π stacking was demonstrated to be an important interaction between MWNT and PI via WAXD and fluorescence emission spectroscopy, and it was influenced by the linkage bond between benzene rings in PIs. This work is of significance to reveal the interfacial features between conjugated polymer and carbon nanotubes (CNTs), which is favorable for the interface design of CNT-based high performance nanocomposites. [ABSTRACT FROM AUTHOR]

In present work, carbon nanomaterials (CNMs) are investigated as potential carriers of 68Ga, which is widely used in positron emission tomography (PET) in nuclear medicine. Sorption behavior of 68Ga was studied onto CNMs of various structures and chemical compositions: nanodiamonds (ND), reduced graphite oxide (rGiO) and multi-walled carbon nanotubes (MWCNT), as well as their oxidized (ND–COOH) or reduced (rGiO–H, MWCNT–H) forms. The physicochemical properties of the nanoparticles were determined by high resolution transmission electron microscopy, x-ray photoelectron spectroscopy, dynamic light scattering and potentiometric titration. The content of 68Ga in the solutions during the study of sorption was determined by gamma-ray spectrometry. The highest degree of 68Ga sorption was observed on ND and ND–COOH samples, and the optimal sorption conditions were determined: an aqueous solution with a pH of 5–7, m/V ratio of 50 μg/mL and a room temperature (25 °C). The 68Ga@ND and 68Ga@ND–COOH conjugates were found to be stable in a model blood solution—phosphate-buffered saline with a pH of 7.3, containing 40 g/L of bovine serum albumin: 68Ga desorption from these samples in 90 minutes was no more than 20% at 25 °C and up to 30% at 37 °C. Such a quantity of desorbed 68Ga does not harm the body and does not interfere with the PET imaging process. Thus, ND and ND–COOH are promising CNMs for using as carriers of 68Ga for PET diagnostics. [ABSTRACT FROM AUTHOR]

Kraft lignin was catalytically graphitized to graphene-based nanostructures at high temperature under non-oxidative atmospheres. To obtain the best catalytic performance, a uniform catalyst–lignin mixture must be made by bonding transitional metal (M) ions to oxygen (O), sulfur (S) or nitrogen (N)-containing functional groups in kraft lignin. One of the strategies is to dissolve or disperse kraft lignin in a suitable solvent, whereby the polymer chains in the condensed lignin molecules will be detangled and stretched out while the functional groups are solvated, and when mixing lignin solution with catalyst metal solution, the solvated metal ions in an aqueous solution can diffuse and migrate onto lignin chains to form M-O, M-S, or M-N bonds during the mixing process. Therefore, solvent effects are important in preparing M–lignin mixture for production of graphene-based nanostructures. Fe–lignin precursors were prepared by dissolving lignin with different solvents, including water, methanol, acetone, and tetrahydrofuran (THF). Solvent effects on the catalytic performance, size and morphology of graphene-based nanostructures were investigated using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), high resolution transmission electron microscopy (HRTEM), and nitrogen sorption measurements. The sizes, morphologies, and catalytic properties of the products obtained from Fe–lignin precursors are greatly influenced by the solvents used. It was found that Fe–lignin (THF) had the highest iron dispersion and the smallest iron particle size. Furthermore, Fe–lignin (THF) exhibited the best catalytic performance for graphitization of kraft lignin while the graphitization degree decreased in the order: Fe–lignin(THF) > Fe–lignin(Acetone) > Fe–lignin(methanol) > Fe–lignin(water). [ABSTRACT FROM AUTHOR]

Spinel gahnite (ZnAl2O4) has been obtained through a hydrothermal synthesis method with a grain size of about 2 nm. The sample was calcined for a few hours at two different temperatures (800 and 900 °C) in order to obtain larger grain sizes to be analyzed by means of powder diffraction with the Rietveld method, and by means of total scattering with the Pair Distribution Function (PDF) method. The idea is to compare the average to the local structure, as a function of increasing grain size. The total scattering data were collected at the European Synchrotron Radiation Facility (ESRF), Grenoble. The samples have been also characterised by means of high resolution Transmission Electron Microscopy (TEM), showing an increasing grain size up to about 9 nm. The average structure presented variations in the inversion degree and an increase in grain size. TEM observations demonstrated that the small crystals are well crystallised: the high resolution images neatly showed the atomic planes, even in the smallest particles. However, the average structure did not properly fit the PDF data in the local region, owing to a slightly different coordination among the octahedra. A new structural model is proposed for the local region of the PDF, that helped our understanding of the differences between a real nanostructured sample and that of a microcrystalline one. The oxygen disorder, due to the inversion grade of the spinel, is demonstrates to be at the basis of the local deviation. No signals of interstitial Zn atoms were detected. [ABSTRACT FROM AUTHOR]