Catalytic properties and electronic structure of copper ions in Cu-ZSM-5

The effect of ion exchange conditions, such as Si/Al ratio, precursor copper salt, pH and concentration of the solution, on the catalytic activity in SCR of NO by propane and on the electronic state of copper ions in Cu-ZSM-5 has been studied. The NO conversion in NO SCR by C₃H₈ has been found to reach a maximum value at Cu/Al ratio about 0.37–0.4 and remain constant at higher Cu/Al.

ESR and UV–vis DR spectroscopy have been used to elucidate stabilization conditions of copper ions in Cu-ZSM-5 zeolites as isolated Cu²⁺ ions, chain copper oxide structures and square-plain oxide clusters. The ability of copper ions for reduction and reoxidation in the chain structures may be responsible for the catalytic activity of Cu-ZSM-5. These transformations of copper ions are accompanied by the observation of intervalence transitions Cu²⁺–Cu⁺ and CTLM of the chain structures in the UV–vis spectra.     

Corrosion Behavior of 316LN and 316 Stainless Steels During Long-term Exposure to Aerated 0.5 M NaCl Using Electrochemical Noise Technique

In the present work 316LN as well as 316 stainless steel (SS) coupons each of dimensions (0.025 × 0.018 × 0.006 m³) in well-polished condition were used as two nominal electrodes which were immersed in the aerated solution of 0.5 M NaCl. Correlated current and potential electrochemical noise (EN) signals were collected at 1 Hz sampling frequency for 1 h daily over a period of 30 days. The detrended EN data were used to calculate the noise resistance (R _N) as well as the spectral noise resistance at zero frequency (R _SN^o) values and other statistical parameters. To study the nature of pits and distribution of their diameters as well as depths, extensive observations of the pitted and the blank specimens were carried out using Confocal Laser Scanning Microscopy (CLSM). The current and the potential records of the two alloys showed distinct differences in their corrosion behavior. It was observed that within less than 4 h of immersion, 316SS showed signals indicative of unstable pitting and onset of stable pitting was noticed after 48 h of exposure. However, until about 24 h, 316LN showed just the random signals and unstable pitting was observed after 28 h. The signals clearly indicated continuous growth of the stable pits in 316SS as against the repassivation of the unstable pits in 316LN after 7 days exposure. It was observed that R _N values showed a continuous decrease in the case of 316SS, but were quite stable in the case of 316LN over the exposure period. Concurrent to these observations it was observed that 316SS specimen was extensively pitted. The frequency distributions of pit diameters as well pit depths were observed to be highest at 10-20 μm and 5-10 μm, respectively. However, pits with as large as 70-80 μm diameter and as deep as 20-25 μm too were observed. No pits were observed in case of 316LN even after 30 days of exposure, an observation that corroborates well with the stable R _N values. Thus, in the present investigation, the long-term tests using EN technique coupled with CLSM studies conclusively prove that many unstable pits initiated in 316SS turn into stable ones resulting in insidious localized corrosion attack whereas the unstable pits initiated in 316LN get passivated in the simulated coastal environment.     

Grain growth kinetics in Dy-doped Bi0.5Na0.5TiO3 ceramics

Dysprosium-doped bismuth sodium titanate ceramics were prepared using the conventional mixed-oxide method. The amount of dysprosium used was varied from 0 to 2 at.%. The mixed powders were calcined at 800 °C and checked for phase purity using X-ray diffraction technique. The calcined powders were then cold-pressed into pellets and sintered at 1050 °C for the time ranging from 2 to 48 h. The ceramics were checked for phases and microstructures using an X-ray diffractometer and a scanning electron microscope, respectively. The analysis showed that undoped BNT ceramics sintered at longer time exhibited a significant grain growth with non-uniform grain size distribution and shape. The Dy-doped BNT however showed a much more limited grain growth behavior, resulting in smaller grain size and more equiaxed grain shape. It was also found that all Dy-doped BNT ceramics sintered at 48 h possessed lower porosity than those sintered for shorter time.     

Life cycle of hydroprocessing catalysts and total catalyst management

Hydroprocessing catalysts based on Ni, Co, Mo and W are used in various refinery processing applications where several deactivation mechanisms become of importance (coke formation, active phase sintering, metals deposition, poisoning) in the catalyst's life cycle. The life cycle of commercial hydroprocessing catalysts is very complex and includes the catalyst production, sulfidation, use, oxidative regeneration followed by re-sulfidation and reuse or, if reuse is not possible, recycling or disposal. To understand the changes in catalyst properties taking place during a life cycle, the catalyst quality in the different stages can be best monitored by using advanced analytical techniques. The catalyst's life cycle is further complicated by numerous technical, environmental and organizational issues involved. In principle, different companies can be involved in each of the life cycle steps. Leading catalyst manufacturers, together with specialized firms, offer refineries a total catalyst management concept, starting with the purchase of the fresh catalyst and ending with its final recycling or disposal. Total catalyst management includes a broad range of services, ensuring optimal timing during the change-out process, reliable, smooth and safe operations, minimal downtime and maximum catalyst and unit performance.     

Signal analysis of total internal reflection fluorescent speckle microscopy (TIR-FSM) and wide-field epi-fluorescence FSM of the actin cytoskeleton and focal adhesions in living cells

Fluorescent speckle microscopy (FSM) uses low levels of fluorescent proteins to create fluorescent speckles on cytoskeletal polymers in high‐resolution fluorescence images of living cells. The dynamics of speckles over time encode subunit turnover and motion of the cytoskeletal polymers. We sought to improve on current FSM technology by first expanding it to study the dynamics of a non‐polymeric macromolecular assembly, using focal adhesions as a test case, and second, to exploit for FSM the high contrast afforded by total internal reflection fluorescence microscopy (TIR‐FM). Here, we first demonstrate that low levels of expression of a green fluorescent protein (GFP) conjugate of the focal adhesion protein, vinculin, results in clusters of fluorescent vinculin speckles on the ventral cell surface, which by immunofluorescence labelling of total vinculin correspond to sparse labelling of dense focal adhesion structures. This demonstrates that the FSM principle can be applied to study focal adhesions. We then use both GFP‐vinculin expression and microinjected fluorescently labelled purified actin to compare quantitatively the speckle signal in FSM images of focal adhesions and the actin cytoskeleton in living cells by TIR‐FM and wide‐field epifluorescence microscopy. We use quantitative FSM image analysis software to define two new parameters for analysing FSM signal features that we can extract automatically: speckle modulation and speckle detectability. Our analysis shows that TIR‐FSM affords major improvements in these parameters compared with wide‐field epifluorescence FSM. Finally, we find that use of a crippled eukaryotic expression promoter for driving low‐level GFP‐fusion protein expression is a useful tool for FSM imaging. When used in time‐lapse mode, TIR‐FSM of actin and GFP‐conjugated focal adhesion proteins will allow quantification of molecular dynamics within interesting macromolecular assemblies at the ventral surface of living cells.     

Nucleation of branches in elastomeric polypropylene

The formation of a crosshatched morphology during crystallization of an isotactic polypropylene with low crystallinity is studied in detail. Here, a lamella seems to grow through another nearly perpendicular lamella that was crystallized before. The crystallization was observed with in situ scanning force microscopy with a temporal resolution of 3 min per image. After crystallization the volume structure was imaged by nanotomography. A detailed scheme for the nucleation of branches is proposed.     

Ennoblement of stainless steel in natural seawater – A new explanation

The ennoblement of corrosion potential (E_corr) of passive metal immersed in seawater was investigated with electrochemical technology and epifluorescence microscopy. The in situ observation showed that the bacteria number increased on the metal surface according to an exponential law which was in the same way with the ennoblement of E_corr. At the same time, the anodic polarization current of high‐Mo stainless steel decreased in the initial days. According to the mix‐potential theory and the characteristics of polarization curves of high‐Mo steel in natural seawater, the ennoblement of corrosion potential may be induced by the decrease of the passive current density.     

Highly oriented star-like patterns observed on GaSe epilayers grown on Si(111)

Epitaxial lamellar gallium selenide (GaSe) semiconductors have been grown on trench-patterned silicon (Si) substrates by molecular beam epitaxy. An intriguing star-like patterned morphology was identified by atomic force microscopy on these epilayers. This non-trivial feature can be correlated with the accumulation of stacking faults of two concurrent epitaxial domains around self-oriented triangular pits developed earlier on the Si(111) surface by the chemical etching. Crystallographic considerations show how the stars can be formed.     

Sintering studies of nano-crystalline zinc oxide

Sintering and grain growth of nano-crystalline undoped ZnO has been studied in detail over a wide range of temperature and holding time. Below 800 °C, sintering of over 70% theoretical density is not observed, irrespective of particle size. At 900 °C for 6 h, the nano-crystalline sample sinters to 99% of theoretical density whereas the density for as received sample is 93% of theoretical density. However, at 1300 °C or higher, the densification is found to be much faster and after a few hours becomes independent of holding time. Grain growth studies reveal a similar feature of attaining saturation over holding time. The average saturated grain size is found to be ∼1.5 and ∼2.2 μm at 800 and 900 °C, respectively, while at 1300 °C or higher, it is in between 12 and 13 μm.