X-Ray Mapping and Interpretation of Scatter Diagrams

Electron beam induced quantitative X-ray mapping has become a very useful characterisation tool for determining the elemental distribution in materials, whether using energy dispersive spectroscopy or wavelength dispersive spectroscopy. The X-ray intensity distributions of the elements from an X-ray map allow us to generate two dimensional and ternary scatter diagrams thus converting spatial information into concentration dimensions, which is an important tool for displaying the spatial relationships of elements or correlated elements (phases) in materials. To best understand how to use this tool, we need to understand the production and features of the scatter diagram. The type of clustering observed in the scatter diagram, whether oval, linear or spherical, can give the major and trace element distributions within phases as well as qualitative and quantitative phase information. This paper demonstrates the generation of scatter diagrams, properties of scatter diagrams, interpretation of scatter diagrams and the advantages of scatter diagrams through the use of examples.     

Liquid crystals based on hypervalent sulfur fluorides: Part 4. [1] Pentafluorosulfanyl alkanes and olefins

New liquid crystals with a pentafluorosulfanyl function as their polar terminal group were prepared and fully characterized. The synthetic key step was the triethyl borane-catalyzed addition of SF₅Br to a suitable olefin precursor, followed by dehydrobromination. The most interesting characteristic of the new materials is their combination of high polarity (Δɛ) with very low birefringence (Δn), which is of particular importance for LCDs for mobile applications.     

A versatile protocol for the preparation of substituted 1- and 2-naphthyl piperazines from aminonaphthols

Aminonaphthols are easily transformed into a variety of 1- and 2-naphthyl piperazines using a sequence of diazotization, iodide substitution and Pd(0) catalyzed coupling reactions.     

Effect of Conditions of Electric-Spark Dispersion of Zinc on the Quality of the Product Obtained

Influence exerted by additives introduced into the working solution, by iron or copper formedin electric-spark dispersion of these metals and zinc, on the quality of the products obtained in electric erosionwas studied.     

Seeded growth of AlN on N- and Al-polar 〈0001〉 AlN seeds by physical vapor transport

We demonstrated seeded growth of AlN on large-area Al- and N-polar <0 0 0 1>-oriented AlN seeds using the physical vapor transport method (PVT). In both cases, crystals having a diameter of 15 mm were obtained from 5 mm seeds. Based on growth step and terrace width analyses, it was found that the N-polar face was suitable for growth within a large window of growth parameters while the Al-polar seeds yielded high-quality crystals only at low supersaturation.     

Decay kinetics of the green emission in tungstates and molybdates

Luminescence characteristics of a number of undoped and variously doped PbWO₄ crystals were studied at 0.4–400 K by the time-resolved spectroscopy and compared with those of ZnWO₄,CdWO₄ and PbMoO₄ crystals. Two types of green emission centres are detected in PbWO₄ crystals. The centres of the first type are responsible for the low-temperature 2.3–2.4 eV emission observed under excitation around 3.90–3.95 eV. The structure and parameters of their relaxed excited states were determined. It was concluded that the origin of defects responsible for the green emission of the first type could vary for different crystals. The centres of the second type with the emission around 2.5 eV appear in crystals containing oxygen vacancies after the thermal destruction of Pb⁺-WO₃ centres at T>180 K. Decomposition of the exciton and various defect-related states was also studied, and activation energies of this process were calculated.     

Electron spin lifetimes in Hg0.78Cd0.22 Te and InSb

We have made direct pump–probe measurements of spin lifetimes in long wavelength narrow-gap semiconductors at wavelengths between 4 and 10 μm and from 4 to 300 K. In particular, we measure remarkably long spin lifetimes, τ_s300 ps, even at 300 K for epilayers of degenerate n-type InSb. In this material the mobility is approximately constant between 77 and 300 K, and we find that τ_s is approximately constant in this temperature range. In order to determine the dominant spin relaxation mechanism we have investigated the temperature dependence of τ_s in non-degenerate lightly n-type Hg_0.78Cd_0.22Te of approximately the same band gap as InSb, and find that τ_s varies from 356 ps at 150 K to 24 ps at 300 K. Our results, both in magnitude and temperature dependence of τ_s, imply that the Elliott–Yafet model dominates in these materials.     

Classical in-plane negative magnetoresistance and quantum positive magnetoresistance in undoped InSb thin films on GaAs (1 0 0) substrates

Magnetoresistance (MR) effects have been investigated in perpendicular and parallel magnetic fields at 300, 80 K and liquid He temperatures for undoped InSb thin films 0.1–2.3 μm thick grown on GaAs(1 0 0) substrates by MBE. At high temperatures, the intrinsic carriers show the parabolic negative MR observable only in magnetic fields parallel to the film. The skipping-orbit effect due to surface boundary scattering in the classical orbits in the plane vertical to the film has been argued to be responsible for the negative MR. At low temperatures (T=80 K), the transport is dominated by the two-dimensional (2D) electrons in the accumulation layers at the InSb/GaAs(1 0 0) hetero interface; MR is positive and shows a logarithmic increase with anisotropy between parallel and perpendicular field orientation, arising from the 2D weak anti-localization (WAL) that reflects the interplay between the spin-Zeeman effect and strong spin–orbit interaction caused by the asymmetric potential at the interface (Rashba term). The zero-field spin splitting energy of Δ₀13 meV, the electron effective mass of m^*0.10m₀ seven times of the band edge mass in bulk InSb and the effective g-factor of |g^*|15 in the accumulation layer have been inferred from fits of MR for the 0.1 μm thick film to the 2D WL theory.     

Recent advances in the analysis of steroid hormones and related drugs.

The development during the last 15 years and the state-of-the-art in the analysis of bulk steroid hormone drugs and hormone-like structures and pharmaceutical formulations made thereof are summarized. Other steroids (sterols, bile acids, cardiac glycosides, vitamins D) as well as biological-clinical aspects and pharmacokinetic and metabolic studies are excluded from this review. The state-of-the-art is summarized based on comparisons of monographs in the latest editions of the European Pharmacopoeia, United States Pharmacopoeia and the Japanese Pharmacopoeia. This is followed by sections dealing with new developments in the methodology for the fields of spectroscopic and spectrophotometric, chromatographic, electrophoretic and hyphenated techniques as well electroanalytical methods. The review is terminated by two problem-oriented sections: examples on impurity and degradation profiling as well as enantiomeric analysis.     

Non-destructive rapid analysis of brominated flame retardants in electrical and electronic equipment using Raman spectroscopy.

Using Raman spectroscopy without any preparation, we analyzed the brominated flame retardant, polybromodiphenyl ethers (PBDEs), which has been prohibited by the European Union. The typical Raman bands of PBDEs, which are clearly different from those of other brominated flame retardants, are from 100 to 300 cm(-1). In our analysis, the detection limit was about 100 ppm, and the analysis took about 1 min, whereas the usual method of solvent extraction using gas chromatography/mass spectroscopy takes 50 h.