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Suite of Python Libraries that implement structure data format processing, multivariate analysis, and interactive visualization of microscopy data and other spectral imaging modalities, including scanning probe microscopy, electron microscopy, Bragg diffraction microscopy, and chemical imaging.
Highlights: • Highly stable gold nanoparticles were synthesized by a simple photochemical process. • TiO{sub 2} nanotubes were used as substrate for preparation of a novel 3D modified electrode. • This electrode was capable of chlorate ion reduction and detection. - Abstract: The present work describes the synthesis, characterization and application of Au nanoparticles modified titanium nanotube electrode (Nano-Au/TiO{sub 2}NT) as a novel and sensitive electrode material for electrochemical sensing of chlorate. For this purpose, highly ordered TiO{sub 2} nanotube (TiO{sub 2}NT) electrode was synthesized by anodization of metallic titanium foil in ethylene glycol-water solution. Nano-Au/TiO{sub 2}NT was obtained by drop casting a solution of homogeneous and fine structures of gold nanoparticles, which were prepared from HAuCl{sub 4} using a new simple photochemical process. Structural and elemental analysis characteristics of the resulting Nano-Au/TiO{sub 2}NT electrode were investigated by scanning electron microscopy and X-ray diffraction analysis. The electrocchemical activity of resulted Nano-Au/TiO{sub 2}NT electrode towards chlorate reduction in acidic solution was confirmed by cyclic voltammetry and chronoamperometry methods An enhancement of amperometric current in the presence of chlorate was afforded to chlorate detection with a low detection limit of 12 μM and linear range of 50 μM to 4.8 mM.
Sorghum was pretreated by sole ultrasound or supercritical carbon dioxide (scCO{sub 2}), as well as the method combining both to intensify enzymatic hydrolysis. The effect of the time (1–5 h) and temperature (30–70 °C) on ultrasonic pretreatment was investigated, and the best condition was determined as 5 h and 50 °C with the EH sugar yield of 33.69%. The influence of the time (6–48 h), temperature (40–80 °C), and pressure (15–25 MPa) on scCO{sub 2} pretreatment were also discussed in this study. The optimum condition of scCO2 pretreatment was identified as 60 °C, 20 MPa, and 36 h with the EH sugar yield of 43.57%. Compared with the sole ultrasonic or scCO{sub 2} pretreatment, scCO{sub 2} associated with the subsequent ultrasonic pretreatment did not show significant improvement in sugar yield. However, 30 MPa was an extremely effective pressure, which led to 45.50% EH sugar yield with 60 °C, 6-h pretreatment. Finally, the change of the microscopic structures of the sorghum stalk after the pretreatment was investigated using scanning electron microscope (SEM) and X-ray diffraction (XRD).
Zinc ultrafine powders (UFPs) with the average particle size of 0.175 to 1.24 μm are synthesized via the flow-levitation method. The peculiarities of the formation of zinc UFPs are considered with respect to the carrier gas properties (heat capacity, thermal conductivity, and diffusion coefficient), as well as the gas flow parameters (pressure and flow rate). The obtained zinc particles are studied via scanning electron microscopy and X-ray diffraction. The factors determining the crystal structure of zinc particles and their size distribution are discussed as well. The data on oxidation of zinc stored in unsealed containers under normal conditions are also presented.
The phase relations in the R{sub 2}Fe{sub 14}B–Y{sub 2}Fe{sub 14}B (R = Nd and Pr) systems have been investigated by means of X-ray powder diffraction (XRD), differential thermal analysis (DTA), and scanning electron microscopy (SEM) equipped with energy-dispersive X-ray spectroscopy (EDS). Crystal structure parameters for all studied alloys (R{sub 1−x}Y{sub x}){sub 2}Fe{sub 14}B (R = Nd and Pr) have been determined by Rietveld refinements. Their structures are similar to that of the Nd{sub 2}Fe{sub 14}B phase with tetragonal structure (space group P4{sub 2}/mnm). The continuous solid solutions are formed in these systems. The lattice parameters and unit cell volumes of the (R{sub 1−x}Y{sub x}){sub 2}Fe{sub 14}B (R = Nd and Pr) solid solutions decrease gradually with increasing Y content. The DTA results present that the decomposition temperature of (R{sub 1−x}Y{sub x}){sub 2}Fe{sub 14}B (R = Nd and Pr) rises with x ranging from 0 to 1.0. The vertical sections of the R{sub 2}Fe{sub 14}B–Y{sub 2}Fe{sub 14}B (R = Nd and Pr) systems are presented in this work.
The dust generated from the basic oxygen steelmaking (BOS) process is a waste material mainly containing iron that cannot be recycled owing to its high zinc content. In this study, the leaching effects of different organic acids are compared, with the aim of determining an acid that selectively leaches and removes zinc from BOS dust, so that the waste material can be recycled into ironmaking and steelmaking processes in order to substitute part of the raw materials of steelmaking. The dust used in this study was scrubbed and collected in the form of a filter cake. The acids tested were oxalic, citric, acetic, propionic, butyric, and valeric acids. Butyric acid was found to be the most effective, with a high zinc extraction level of 49.7 pct and a low iron level of only 2.5 pct. Oxalic acid was the least effective leaching reagent for both zinc and iron extractions, owing to the formation of zinc and iron oxalate precipitates following metal dissolution. The filter cake and leached residues were characterized by chemical analysis, X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy with energy dispersive spectroscpopy.
The strength retrogression of a Class G cement enriched by adding 60–80% silica cured under the condition of 200 °C and 50 MPa were investigated by multiple different analysis methods. Short-term strength analysis suggests sonic strength testing is a poor indicator of real mechanical strength at such curing condition. Long-term testing up to 142 d shows all designed systems experiences dramatic deterioration in physical and mechanical properties, such as compressive strength, Young's modulus, water permeability and gas permeability. Further testing was conducted using X-ray diffraction, thermal gravimetric analysis, mercury intrusion and scanning electron microscope. The study reveals that the set cement experiences significant microstructure coarsening with increasing curing time, especially after 30 d curing. The strength retrogression and microstructure coarsening seem to be accompanied with the continued consumption of silica, and are likely caused by the gradual conversion of semi-crystalline C-S-H into crystalline tobermorite and xonolite over the long-term curing.
Highlights: • Birnessite-type MnO{sub 2} nanoparticles were prepared by the microwave-assisted reflux. • The microwave reaction duration was only 5 min. • A specific capacitance of 329 F g{sup −1} was obtained for birnessite-type MnO{sub 2}. - Abstract: Birnessite-type MnO{sub 2} nanoparticles have been successfully synthesized by the microwave-assisted reflux as short as 5 min. The microstructure and morphology of the products were characterized by X-ray diffraction, N{sub 2} adsorption–desorption isotherms, scanning electron microscopy, transmission electron microscopy. The electrochemical properties of the as-prepared MnO{sub 2} as an electrode material for supercapacitor were investigated by cyclic voltammetry and galvanostatic charge-discharge measurements in 1 M Na{sub 2}SO{sub 4} electrolyte, and a high specific capacitance of 329 F g{sup −1} was achieved at a current density of 0.2 A g{sup −1}. The specific capacitance retention was 92% after 1000 cycles at 2 A g{sup −1}, suggesting that it is a promising electrode material for supercapacitors.
Highlights: • CdSe nanowires were prepared by template assisted electro-deposition. • CdSe nanowires were implanted with 200 keV P{sup −} ions at different fluence. • Structure of CdSe NWs remained intact on ion implantation. • Optical band gap of CdSe NWs decreased after implantation. • The electrical conduction improved due to dominance of ionization effects. - Abstract: For II–VI compound semiconductor nanostructures, ion implantation is considered to be an area of significant interest due to its potential use in the fabrication of the extensive variety of novel optoelectric devices. CdSe nanowires with diameter 80 nm have been grown via the template-assisted electro-deposition method and were subsequently implanted with 200 keV negative phosphorous ions at fluence ranging from 10{sup 11} ions/cm{sup 2} to 10{sup 13} ions/cm{sup 2}. SRIM-TRIM simulation studies are done to understand the course and nature of events occurring during implantation. Pre- and post-implanted samples were characterized by Scanning electron microscope (SEM), X-Ray diffraction (XRD), UV–vis spectroscopy and Probe station with a Keithley source meter. Structural studies reveal no modification in crystal structure upon implantation. An increase of phosphorous content led to an apparent red shift in the optical band gap and an improvement in conductivity. These modifications are attributed to the ionization and the creation of damage on implantation.
The modification of the fly ash (FA) by magnetite (M) was performed to obtain FAM adsorbent with improved adsorption efficiency for arsenate removal from water. The novel low cost adsorbents are characterized by liquid nitrogen porosimetry (BET), scanning electron microscopy (SEM), X-ray diffraction (XRD), Mössbauer spectroscopy (MB) and Fourier transform infrared (FTIR) spectroscopy. The optimal conditions and key factors influencing the adsorbent synthesis are assessed using the response surface method (RSM). The adsorption experiment was carried out in a batch system by varying the contact time, temperature, pH, and mass of the adsorbent. The adsorption capacity of the FAM adsorbent for As(V), calculated by Langmuir model, was 19.14 mg g−1. The thermodynamic parameters showed spontaneity of adsorption with low endothermic character. The kinetic data followed the pseudo-second-order kinetic model (PSO), and Weber-Morris model indicated intra-particle diffusion as rate limiting step. Alternative to low desorption capability of the FAM was found by five consecutive adsorption/magnetite precipitation processes which gave exhausted layered adsorbent with 65.78 mg g−1 capacity. This research also has shed light on the mechanism of As(V)-ion adsorption, presenting a promising solution for the valorization of a widely abundant industrial waste. © 2018 Elsevier Ltd.
The effects of solutionizing soak time and aging on the microstructure and mechanical properties of cast AZ80 Mg alloy were investigated. Optical microscopy, scanning electron microscopy and x-ray diffraction revealed the dissolution of β-Mg{sub 17}Al{sub 12} phase in the solution-treated samples which was later detected in the aged condition. Solution treatments at 420 °C for 4-16 h with water quenching followed by aging at 200 °C for 10 h were carried out, causing discontinuous precipitates to be formed with different precipitate morphologies at the various soak times. The discontinuous precipitates were observed to transform from the interdendritic segregation to parallel lamellae with increasing soak time to 8-10 h. As the soak time increased to 16 h, parallel lamellae transformed into tree-like precipitate morphology. The results showed significant changes in the interlamellar spacing at different soak times, and such precipitate morphology could influence the microstructure and mechanical properties after the aging process. A good combination of strength and ductility was obtained when the cast AZ80 Mg alloy was solution-treated at 420 °C for 10 h and aged at 200 °C for 10 h. Compared to the as-cast condition, a significant increase in ultimate tensile strength (50%), yield strength (47%) and elongation (43%) were observed.
The selective modification of sodium montmorillonite (Na{sup +}-Mt) surface with polyionene followed by poly (succinimde-co-aspartate) has been considered. Na{sup +}-Mt was allowed to react with well characterized polyionene in two fold excess. The resulting polyionene/Mt (IC) was further modified with poly (succinimide-co-aspartate) through an ion exchange process. The obtained polyaspartate/Mt (IPS) composite was characterized by elemental analysis, X-ray diffraction, FTIR spectroscopy, thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and BET surface analyzer. The adsorption efficiency of IPS composite was investigated for the removal of Pb(II) and Cd(II) from aqueous solution under different experimental conditions including initial metal ions concentration, temperature and single and binary mixture systems of metal ions. The experimental data were analyzed by Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich models. Langmuir model reveals that the monolayer adsorption capacity of IPS was 92.59 and 67.57 mg/g for Pb(II) and Cd(II), respectively. The modification of parent Na{sup +}-Mt enhanced their adsorption capacity by about 87.91 and 29.84% for Pb(II) and Cd(II), respectively, due to inclusion of extra active sites of polyaspartate. The mean sorption energy, E calculated from Dubinin–Radushkevich isotherm were 2.75 and 1.98 kJ/mol for the adsorption of Pb(II) and Cd(II), respectively, indicating physical adsorption process. Also, The thermodynamic parameters were calculated and indicated that the adsorption was spontaneous and exothermic process. The mechanism of cation exchange and complexation of metal ions was suggested. IPS composite has a considerable potential for the removal of heavy metal ions from aqueous solution and wastewater stream.
In this study, the wear properties of in-situ 7075 Al-Ti composites produced by powder metallurgy route were investigated. Different amount of Ti (2, 4, 6 %) added to gas atomized 7075 Al alloy powders and they were mixed in turbula with 47rpm for 45 minutes. Then the mixed powders were pre-shaped by press under 600 MPa pressure. The samples were cooled in the furnace after sintered at 580 °C for 4 hours in the atmosphere controlled furnace. Standard metallographic process such as grinding, polishing and etching were applied to sintered samples. The hardness values were measured. Scanning Electron Microscope (SEM), X-Ray Diffraction (XRD) examines were carried out. The wear tests were performed in a pin-on disc type wear apparatus with 1 ms{sup −1} sliding speed at six different sliding distance (500-3000 m) under 30 N loads. As a result of studies, hardness values were increased with increasing Ti content, in addition the weight losses were decreased with increasing Ti amount.
Graphical abstract: Polypyrrole(PPy) film has improved the rate performance of LiMn{sub 2}O{sub 4} efficiently due to its excellent conductivity. PPy@LiMn{sub 2}O{sub 4} could provide more energy under the higher power than pristine LMO. - Highlights: • The PPy layer on the surface of LMO particles hasn’t been studied in LiMn{sub 2}O{sub 4} so far. • The solvent in the synthesis process of PPy@LMO is absolute ethyl alcohol. • The differences of surface-modification between the PPy and PI for LMO. • The analyses of rate performances are through specific power. - Abstract: Polypyrrole (PPy) is an excellent conductive polymer and the study on its utilization in the surface modification of the LiMn{sub 2}O{sub 4} (LMO) is few. In this work, the structure, morphology and electrochemical performance of surface-modified LiMn{sub 2}O{sub 4} composites with PPy and polyimides (PI) were discussed. The crystal structure, chemical bonds and morphology were characterized through X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM), respectively. Moreover, the specific power and cycling performance were tested at room and high (55 °C) temperature. The PPy@LMO (surface-modified LMO composites with PPy) shows better performances than the pristine LMO. The addition of PPy not only weakens the corrosion caused by electrolyte, but also improves the discharge capacity at higher rates. The charge transfer resistance of the PPy@LMO is much lower than that of the pristine LMO after cycling.
Highlights: • A hydrothermal route to m-LaVO{sub 4}/BiOBr composite photocatalysts was proposed. • Products exhibit excellent photocatalytic activity under visible light. • Enhanced photocatalytic activity can be ascribed to forming p-n heterojunction. - Abstract: Visible-light driven m-LaVO{sub 4}/BiOBr composite photocatalysts were synthesized by a two-step hydrothermal process, and were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), photoluminescence spectroscopy (PL), and UV–vis diffuse reflectance spectroscopy, respectively. The results showed that 1.0 wt% LaVO{sub 4}/BiOBr sample exhibits the highest photodegradation rate of RhB under visible-light irradiation, within 60 mins, it achieved 83.37%. The enhanced photocatalytic performance can be ascribed to the formation of p-n heterojunction structure and the inhibition of m-LaVO{sub 4} to 2D growth of BiOBr to a certain extent.
We report on the molecular beam epitaxy growth and characterization of TbAs films. In situ reflection high energy electron diffraction and ex situ high resolution X-ray diffraction, reciprocal space mapping, and both scanning and transmission electron microscopy are used to confirm the complete film growth and study the films’ morphology. Spectrophotometry measurements provide the energy of optical transitions, revealing a red shift in optical band gap with increasing thickness. The Hall effect measurements show temperature insensitive carrier concentrations, resistivities, and mobilities. The carrier concentration decreases and resistivity increases with increasing film thickness; mobility appears thickness independent. Here, the films’ reflectivity, obtained via Fourier transform infrared spectroscopy, shows a possible Drude edge that differs from the trend of other lanthanide monopnictides. Lastly, these measurements show that TbAs is a degenerately doped semiconductor with a combination of electronic and optical properties that is dissimilar to other lanthanide monopnictides.
SrTi{sub 1−x}Fe{sub x}O{sub 3} (x = 0, 0.05 and 0.1) nanofibers (NFs) were fabricated by electrospinning technique. As prepared products were calcined at 800 {sup ∘} C in argon atmosphere for 3 h to obtain a perovskite phase. The crystal structure and morphology of samples were investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Electrochemical and magnetic properties of calcined NFs were studied using a potentiostat/galvanostat electrochemical cell system and vibrating sample magnetometer (VSM), respectively. XRD results showed the cubic perovskite structure of calcined samples with the diameter estimated by TEM in the range of 137.4–141.3 nm SEM micrographs revealed the linkage of crystalline grains in NFs of porous and rough surfaces. Electrochemical properties performed on coin-cell-type Li-ion batteries (LIBs) with calcined SrTi{sub 1−x}Fe{sub x}O{sub 3} (x = 0.05 and 0.10) NF-based anodes showed a significant increase of the specific capacity from 305 to 431 mAh/g for the first cycle with the reversible values of 100 and 130 mAh/g, respectively. VSM measurements at room temperature (RT) indicated that calcined SrTiO{sub 3} NFs exhibited paramagnetic (PM) behavior, while calcined SrTi{sub 1−x}Fe{sub x}O{sub 3} NFs displayed ferromagnetic (FM) behavior at RT with the increase of unsaturated magnetization at 10 kOe from 0.46 to 0.82 emu/g for samples with x = 0.05 and 0.10, respectively. The observed FM behavior in calcined SrTi{sub 1−x}Fe{sub x}O{sub 3} (x = 0.05 and 0.1) NFs was suggested to originate from the face center exchange (FCE) mechanism owing to Fe{sup 3+} –Vo–Fe{sup 3+} couplings.
Highlights: • Pure quasi-stoichiometric CTS nanoparticles obtained by green hydrothermal route. • Cubic structure of CTS nanoparticles without secondary phases was acheived. • A formation mechanism of the CTS nanoparticles is proposed. • CTS has a band gap of Eg = 1.4 eV, which is optimal for photovoltaïc absorber. - Abstract: In this study, nanoparticles of Cu{sub 2}SnS{sub 3} (CTS) have been synthesized by a simple one-step hydrothermal route without annealing. Metal chlorides and sodium sulphide precursors were dissolved in green solvent (water) and maintained at 230 °C for 24 h in a laboratory scale autoclave. Structural, morphological and optical characterization of synthesized CTS nanoparticles has been performed by Energy Dispersive Spectrometry (EDS), X-Ray Diffraction (XRD), Raman Spectroscopy, Field Emission Scanning Electron Microscopy (FESEM), Transmission Electron Microscopy (TEM) and UV–vis-NIR Spectroscopy. The results appear to confirm the formation of pure and quasi-stoichiometric cubic CTS nanoparticles. No secondary phases have been detected. The average size of the synthesized nanoparticles is estimated to be about 30 nm. From the absorption measurements, the optical band gap energy of the CTS nanoparticles was estimated to be 1.4 eV. This is very close to the optimal value required for an absorber material in photovoltaic (PV) solar energy conversion. In order to improve the understanding of the formation mechanism of CTS nanoparticles, the precipitate recovered prior to the hydrothermal reaction was analysed by EDS and XRD. The obtained results suggest that the formation of CTS nanoparticles takes place in two stages. Firstly, it is initiated from the formation of precipitates of Cu{sub 2}S, CuS and SnS binary compounds in the starting precursors solution prior to the hydrothermal reaction and thereafter it is completed under hydrothermal conditions. This study shows the feasibility of synthesizing CTS nanoparticles with abundant elements using an environmentally-friendly and low cost process.