An improved approach for hydrogen analysis in metal samples using single laser-induced gas plasma and target plasma at helium atmospheric pressure

We report in this paper the results of an experimental study on hydrogen analysis of solid samples in high pressure helium ambient gas employing the basic scheme of laser induced breakdown spectroscopy (LIBS). It is shown that the metastable excited state of helium atom can be utilized to induce delayed excitation of the ablated hydrogen atoms, and thereby avoid the Stark broadening effect as well as overcoming the undesirable mismatch effect, which are responsible for inefficient excitation respectively. It is further demonstrated that for samples of high boiling-point materials such as zircaloy, successful hydrogen analysis can be achieved by a newly introduced double excitation technique employing single laser realized in a modified configuration of the conventional LIBS method. PACS 51-52     

Spatially resolved Raman spectroscopy evaluation of residual stresses in 3C-SiC layer deposited on Si substrates with different crystallographic orientations

Raman scattering studies were performed on hot-wall chemical vapor deposited (heteroepitaxial) silicon carbide (SiC) films grown on Si substrates with orientations of (1 0 0), (1 1 1), (1 1 0) and (2 1 1), respectively. Raman spectra suggested that good quality cubic SiC single crystals could be obtained on the Si substrate, independent of its crystallographic orientation. Average residual stresses in the epitaxially grown 3C-SiC films were measured with the laser waist focused on the epilayer surface. Tensile and compressive residual stresses were found to be stored within the SiC film and in the Si substrate, respectively. The residual stress exhibited a marked dependence on the orientation of the substrate. The measured stresses were comparable to the thermal stress deduced from elastic deformation theory, which demonstrates that the large lattice mismatch between cubic SiC and Si is effectively relieved by initial carbonization. The confocal configuration of the optical probe enabled a stress evaluation along the cross-section of the sample, which showed maximum tensile stress magnitude at the SiC/Si interface from the SiC side, decreasing away from the interface in varied rate for different crystallographic orientations. Defocusing experiments were used to precisely characterize the geometry of the laser probe in 3C-SiC single crystal. Based on this knowledge, a theoretical convolution of the in-depth stress distribution could be obtained, which showed a satisfactory agreement with stress values obtained by experiments performed on the 3C-SiC surface.     

Dynamics of molybdenum nano structure formation on the TiO2(1 1 0) surface: A kinetic Monte Carlo approach

The rutile TiO₂(1 1 0) surface is a highly anisotropic surface exhibiting “channels” delimited by oxygen rows. In previous experimental and theoretical DFT works we could identify the molybdenum adsorption sites. They are located inside the channels. Moreover, experimental studies have shown that during subsequent annealing after deposition, special molybdenum nano structures can be formed, especially two monolayer high pyramidal chains of atoms.In order to better understand the dynamics of nano structure formation, we present a kinetic Monte Carlo study on diffusion and adsorption of molybdenum atoms on a TiO₂(1 1 0) surface. A quasi one-dimensional lattice gas model has been used which describes the possible adsorption sites of a Mo atom in a single channel of the surface. The atomic positions of a 1.5 monolayer thick Mo film formed of pyramidal chains define the lattice sites of the model. Thereby the formation of three-dimensional clusters could be studied. Here we have studied the cluster formation as a function of parameters that can be controlled in a growth experiment by physical vapor deposition: deposition and annealing temperature, flux and total amount of deposited Mo. Good qualitative agreement with recent experiments is obtained.     

High-density plasma etching of indium-zinc oxide films in Ar/Cl2 and Ar/CH4/H2 chemistries

The dry etching characteristics of transparent and conductive indium-zinc oxide (IZO) films have been investigated using an inductively coupled high-density plasma. While the Cl₂-based plasma mixture showed little enhancement over physical sputtering in a pure argon atmosphere, the CH₄/H₂/Ar chemistry produced an increase of the IZO etch rate. On the other hand, the surface morphology of IZO films after etching in Ar and Ar/Cl₂ discharges is smooth, whereas that after etching in CH₄/H₂/Ar presents particle-like features resulting from the preferential desorption of In- and O-containing products. Etching in CH₄/H₂/Ar also produces formation of a Zn-rich surface layer, whose thickness (∼40 nm) is well-above the expected range of incident ions in the material (∼1 nm). Such alteration of the IZO layer after etching in CH₄/H₂/Ar plasmas is expected to have a significant impact on the transparent electrode properties in optoelectronic device fabrication.     

Surface and interfacial properties of PVDF/acrylic copolymer blends before and after UV exposure

Morphological and chemical properties of both the surface and interface of poly(vinylidene fluoride)/poly(methyl methacrylate)-co-poly(ethyl acrylate) (PVDF/PMMA-co-PEA) blend films have been investigated before and after the samples were exposed to ultraviolet (UV) irradiation using a xenon arc lamp at 50 °C and 9% relative humidity (RH) for 7 months. Surface and interfacial morphologies were studied by atomic force microscopy (AFM). Chemical composition information was obtained by confocal Raman microscopy, attenuated total reflection-FTIR spectroscopy (ATR-FTIR), X-ray photoelectron spectroscopy (XPS), and contact angle measurements. Results show an enrichment of the PVDF material at the air surface, while the acrylic copolymer enriches the interface. Blends having greater than 50% mass fraction of PVDF show little change in the surface morphology after UV exposure for 7 months. However, for a lower PVDF content, blends exhibit significant degradation of PMMA-co-PEA copolymer and a much rougher surface after UV exposure. Microstructural changes in the PVDF spherulites are also observed after UV degradation. It is found that the surface and interfacial morphologies are correlated with the chemical properties.     

Measurements of theg-factor ratio of the first 3− and 5− states in40Ca and the lifetime of the 5− state

[Theg-factor ratio of the first excited 3^? and 5^? states in⁴⁰Ca was measured to beg ₃/g ₅=1.01(10) employing the implantation perturbed angular correlation technique. The static hyperfine fields (SF) in Fe and Gd hosts were used. In addition the lifetime of the 5^? state was measured to be τ=426(7)ps. The values of the SF in Gd and Fe hosts were deduced and compared with systematics in this element region.     

New methods for determining the volumetric flow rate in the column and the retention time of the unretained substance in gas chromatography

New methods for calculating the mean volumetric flow rate of the carrier gas and the retention time of the unretained substance in the column under conditions of gas chromatography were proposed. The methods are based on preliminary isothermal calibrations of the flow rate and holdup time for a packed column. A theoretical substantiation of the methods was given. Procedures of plotting calibration dependences for determining the indicated quantities at a desired temperature were described. The calculation results were compared to experimental data obtained by traditional methods. It was demonstrated that the use of calculation methods substantially simplifies the determination of the specific retention volume over a wide temperature range.