Electronic structure of Mo1-x Re x alloys studied through resonant photoemission spectroscopy.

We studied the electronic structure of Mo-rich Mo1-x Re x alloys ([Formula: see text]) using valence band photoemission spectroscopy in the photon energy range 23-70 eV and density of states calculations. Comparison of the photoemission spectra with the density of states calculations suggests that, with respect to the Fermi level E F, the d states lie mostly in the binding energy range 0 to -6 eV, whereas s states lie in the binding energy range -4 to -10 eV. We observed two resonances in the photoemission spectra of each sample, one at about 35 eV photon energy and the other at about 45 eV photon energy. Our analysis suggests that the resonance at 35 eV photon energy is related to the Mo 4p-5s transition and the resonance at 45 eV photon energy is related to the contribution from both the Mo 4p-4d transition (threshold: 42 eV) and the Re 5p-5d transition (threshold: 46 eV). In the constant initial state plot, the resonance at 35 eV incident photon energy for binding energy features in the range E F (BE = 0) to -5 eV becomes progressively less prominent with increasing Re concentration x and vanishes for x > 0.2. The difference plots obtained by subtracting the valence band photoemission spectrum of Mo from that of Mo1-x Re x alloys, measured at 47 eV photon energy, reveal that the Re d-like states appear near E F when Re is alloyed with Mo. These results indicate that interband s-d interaction, which is weak in Mo, increases with increasing x and influences the nature of the superconductivity in alloys with higher x.

Optical properties of zirconium carbide in 60-200 Å wavelength region using x-ray reflectivity technique.

Optical constants of zirconium carbide (ZrC) have been determined in the soft x-ray region of 60-200 Å wavelength using angle-dependent x-ray reflectivity measurements. Reflectivity measurements are carried out at the reflectivity beamline of the Indus-1 synchrotron radiation source. Derived optical constants (δ and ß) are compared with the tabulated values [At. Data Nucl. Data Tables 54, 181 (1993)]. The optical constants are 15%-35% lower than bulk values in the 60-200 Å wavelength region. Near the Zr M4 edge 187 eV (66.3 Å), the δ values were close to bulk values with a deviation of 5%-10%. A large deviation of ∼20% was found in beta values especially near the Zr M4 edge region, whereas it was in close agreement in the wavelength range away from the edge. To the best of our knowledge, this paper gives the first reported experimental values of optical constants for zirconium carbide in the 60-200 Å wavelength region.

Determining chemically and spatially resolved atomic profile of low contrast interface structure with high resolution.

We present precise measurements of atomic distributions of low electron density contrast at a buried interface using soft x-ray resonant scattering. This approach allows one to construct chemically and spatially highly resolved atomic distribution profile upto several tens of nanometer in a non-destructive and quantitative manner. We demonstrate that the method is sensitive enough to resolve compositional differences of few atomic percent in nano-scaled layered structures of elements with poor electron density differences (0.05%). The present study near the edge of potential impurities in soft x-ray range for low-Z system will stimulate the activity in that field.

Analysis of higher harmonic contamination with a modified approach using a grating analyser.

Soft x-ray spectra of the toroidal grating monochromator (TGM) at the reflectivity beamline of Indus-1 synchrotron source are analyzed for higher harmonic contribution. A diffraction grating of central line spacing 1200 l/mm is used to disperse the monochromatic beam received from TGM to quantify the harmonic contents in the 50-360 Å wavelength range. In order to calculate the harmonic contamination, conventionally the intensity of higher order peak is divided by first order peak intensity of the desired wavelength. This approach is found to give wrong estimate as first order peak itself is overlapped by higher order peaks. In the present study, a modified approach has been proposed to calculate harmonic contamination where the intensity contributions of overlapping orders have been removed from the first order diffraction peak of the desired wavelength. It is found that the order contamination in the TGM spectra is less than 15% in the wavelength range of 90-180 Å. The total harmonic contribution increases from 6%-60% in the wavelength range of 150-260 Å. The critical wavelength of Indus-1 is 61 Å hence the harmonic contamination below 90 Å is significantly low. The results obtained with modified approach match well with those obtained by quantitative analysis of multilayer reflectivity data. The obtained higher harmonics data are used to fit the transmission of aluminum edge filter in the 120-360 Å wavelength range.

Beamline BL-07 at Indus-2: a facility for microfabrication research.

The X-ray lithography beamline on Indus-2 is now operational, with two modes of operation. With a pair of X-ray mirrors it is possible to tune the energy spectrum between 1 and 20 keV with a controlled spectral bandwidth. In its 'no optics' mode, hard X-rays up to 40 keV are available. Features and performance of the beamline are presented along with some example structures. Structures fabricated include honeycomb structures in PMMA using a stainless steel stencil mask and a compound refractive X-ray lens using a polyimide-gold mask in SU-8.

Study on effective cleaning of gold layer from fused silica mirrors using nanosecond-pulsed Nd:YAG laser.

A study on effective laser cleaning of gold layer deposited on fused silica substrates used in beamlines of synchrotron radiation (SR) sources using nanosecond-pulsed Nd:YAG laser has been carried out. The influence of pulse duration, beam incidence angle, spot overlapping, laser fluence, and number of passes on cleaning efficiency has been investigated. An approximately 48 nm thick gold layer from a mirror surface area of ~48 cm2 has been cleaned in 3 min. Laser clean quality and efficiency has been analyzed using microscope, scanning electron microscope (SEM), and angle-dependent reflectivity measurement techniques using SR beamline. Optimization of cleaning parameters resulted in a cleaning efficiency of ~98%. This study provides an alternate and low-cost solution for reuse of gold-coated, damaged mirrors.

Stability and normal incidence reflectivity of W/B4C multilayer mirror near the boron K absorption edge.

A multilayer structure consisting of alternate layers of W and B4C has been deposited using a magnetron sputtering system. The structure of the as-deposited and vacuum-annealed W/B4C multilayer sample has been characterized using grazing incidence x-ray reflectivity, grazing incidence diffraction, and the normal incidence reflectivity has been measured using synchrotron radiation. A two-layer model consisting of tungsten and boron carbide is presented. The multilayer structure was found to be stable after 800°C annealing. Grazing incidence x-ray diffraction measurements suggested that W is polycrystalline with small grain size. No signature of tungsten carbide or tungsten boride formation could be observed during the annealing treatments. A near normal incidence soft x-ray reflectivity (SXRR) of ~8.3% was obtained at 6.8 nm wavelength. A little drop (~1%) in SXRR after 800°C annealing suggested that there were no compositional changes within the layers during the annealing treatments.

A microfocus X-ray fluorescence beamline at Indus-2 synchrotron radiation facility.

A microfocus X-ray fluorescence spectroscopy beamline (BL-16) at the Indian synchrotron radiation facility Indus-2 has been constructed with an experimental emphasis on environmental, archaeological, biomedical and material science applications involving heavy metal speciation and their localization. The beamline offers a combination of different analytical probes, e.g. X-ray fluorescence mapping, X-ray microspectroscopy and total-external-reflection fluorescence characterization. The beamline is installed on a bending-magnet source with a working X-ray energy range of 4-20 keV, enabling it to excite K-edges of all elements from S to Nb and L-edges from Ag to U. The optics of the beamline comprises of a double-crystal monochromator with Si(111) symmetric and asymmetric crystals and a pair of Kirkpatrick-Baez focusing mirrors. This paper describes the performance of the beamline and its capabilities with examples of measured results.

NbC/Si multilayer mirror for next generation EUV light sources.

In the present study we report a new multilayer combination comprised of refracting layers of niobium carbide and spacer layers of silicon as a more stable and high reflecting combination for the 10 - 20 nm wavelength region. The reflectivity of the new combination is comparable to Mo/Si conventional mirrors. Annealing experiments carried out with NbC/Si multilayer at 600°C temperature showed a ~2.5% drop in the soft x-ray reflectivity along with a marginal contraction in the multilayer period length. The multilayer structure is found stable after the heat treatment. Crystallization of the niobium carbide and silicon layers is responsible for the compaction in the period length as revealed by the grazing incidence x-ray diffraction measurements. No signature of silicide formation or any other chemical species could be detected. The multilayer structures were grown by ion beam sputtering technique using a compound target of niobium carbide. Soft x-ray reflectivity measurements performed at the Indus-1 and BESSY-II synchrotron radiation sources are found in good agreement with the simulations.

Quantitative determination of higher harmonic content in the soft x-ray spectra of toroidal grating monochromator using a reflection multilayer.

Use of a grating monochromator causes a problem of higher harmonic contaminations in a synchrotron beamline operating in the soft x ray/vacuum ultraviolet region. Generally gratings are used to experimentally determine the higher harmonic contaminations. In this method, the relative contribution of contaminant wavelengths is measured with respect to the first harmonic wavelength (desired wavelength). The quantitative fit of grating spectra is rather complex, and therefore qualitative analysis is carried out. Analysis of multilayer reflectivity data has become rather simple with recent advances in the theoretical modeling. Therefore we propose to use a multilayer mirror and analyze its reflectivity data for quantitative determination of harmonic contamination in a soft x ray beamline. In the present study we used a Mo/Si multilayer of d=97 Å to quantify the spectral purity of 600 lines/mm toroidal grating at the reflectivity beamline of Indus-1 450 MeV synchrotron source. The measured reflectivity spectra at each wavelength is analyzed and the actual contribution of higher harmonics in the incident beam is obtained. Details of methodology and results are discussed.

Origin of step-like behavior in the Co/Si system.

A systematic investigation of the structure, nature of the interface and their possible connections with magnetic properties for the as-deposited Co/Si/Co trilayer system has been carried out. X-ray reflectivity, cross-sectional transmission electron microscopy and x-ray emission measurements performed on the Co/Si/Co trilayer system show that when the Si layer thickness is less than ∼ 20 Å, the full Si layer is converted into a cobalt silicide layer whereas when the Si layer thickness > 20 Å along with the silicide layer. the pure Si layer also remains. A comparison of magneto-optical Kerr effect and magnetoresistance measurements reveals the absence of antiferromagnetic coupling in these samples. Double-step-like magnetization, in the case of Si layer thickness > 20 Å between two Co layers, is explained by magnetization reversal of two ferromagnetic layers having different coercivities, independent of each other.

Optical properties of indium phosphide in the 50-200 Å wavelength region using a reflectivity technique.

The optical constants of indium phosphide (InP) in the soft x-ray region of 50-200 Å are determined from angle-dependent reflectivity measurements. The measurements are carried out using the reflectivity beam line at the Indus-1 synchrotron source. The derived optical constants are compared with tabulated values of Henke et al. [At. Data Nucl. Data Tables 54, 181 (1993)]. Experimental values of δ and ß are in close agreement with the tabulated values in the lower wavelength region of 50-120 Å. The experimental value indicates an edge shift of 0.4 Å toward the lower wavelength side from the phosphorous L-edge value of 92 Å. However, above the 120 Å region, where the indium N(2) edge falls at 160.7 Å, there is a huge difference between experimental and tabulated values. Both delta and beta values are significantly higher. In contrast to tabulated values of the ß/δ ratio, which is more than 1 above the 140 Å region, the experimental measured ratio is found to be less than 1. This study presents the first reported experimental values of optical constants for InP in this wavelength range, to the best of our knowledge.

Effect of energy dependence of primary beam divergence on the X-ray standing wave characterization of layered materials.

Incident primary beam divergence is a source of systematic error in X-ray standing wave (XSW) characterization of single and multilayer thin films. Primary beam divergence significantly alters the XSW profile of a layered material and can lead to large errors when used with higher excitation energies. The present study suggests that when one uses Mo-Kalpha excitation, the primary beam divergence should be in range of 0.005(0). On the other hand, in the case of Cu-Kalpha excitation, primary beam divergence can be relaxed up to 0.01(0).

Effect of surface roughness and subsurface damage on grazing-incidence x-ray scattering and specular reflectance.

Grazing-incidence specular reflectance and near-specular scattering were measured at Al-K(alpha) (1.486-keV, 8.34-?) radiation on uncoated dielectric substrates whose surface topography had been measured with a scanning probe microscope and a mechanical profiler. Grazing-incidence specular reflectance was also measured on selected substrates at the Cu-K(alpha) (8.047-keV, 1.54-?) wavelength. Substrates included superpolished and conventionally polished fused silica; SiO(2) wafers; superpolished and precision-ground Zerodur; conventionally polished, float-polished, and precision-ground BK-7 glass; and superpolished and precision-ground silicon carbide. Roughnesses derived from x-ray specular reflectance and scattering measurements were in good agreement with topographic roughness values measured with a scanning probe microscope (atomic force microscope) and a mechanical profiler that included similar ranges of surface spatial wavelengths. The specular reflectance was also found to be sensitive to the density of polished surface layers and subsurface damage down to the penetration depth of the x rays. Density gradients and subsurface damage were found in the superpolished fused-silica and precision-ground Zerodur samples. These results suggest that one can nondestructively evaluate subsurface damage in transparent materials using grazing-incidence x-ray specular reflectance in the 1.5-8-keV range.

Characterization of substrates for use in X-ray multilayer optics.

The optical performance of platinum-carbon multilayers deposited onto different substrates has been examined. Specular reflectivity and non-specular diffuse scattering were measured to study the replication of substrate roughness into the multilayer structure. Surface topography was measured before and after deposition using a scanning probe microscope and a mechanical profiler.

Fabrication and characterization of multilayer supermirrors for hard X-ray optics.

Multilayer supermirrors stacked with three sets of Pt/C combinations have been fabricated on a flat float-glass and conical replica foil mirror using a magnetron DC sputtering system, and applied to X-ray optical systems in the hard X-ray region. The design of the supermirror is optimized to obtain the highest integrated reflectivity in the energy band and at the grazing angle concerned. X-ray reflectivities of 30% in the 25-35 keV band at an incidence angle of 0.3 degrees were obtained.

Energy-dispersive X-ray fluorescence spectrometry technique as an efficient monitoring tool for mercury contamination.

This paper illustrates the useful early-warning role of the energy-dispersive X-ray fluorescence technique against a potential health hazard being posed by dumping effluents from an industrial unit involved in the manufacture of lead-batteries, in a nearby water-canal used for irrigation purposes by surrounding villages. These effluents were shown to contain mercury at a potentially unsafe level, resulting in timely initiation of necessary preventive measures. The standard fundamental parameter method was invoked for a quantitative estimation of the mercury (Hg) concentration. In addition, L-series (rather than the usual K-series) X-rays were used for excitation, mainly on account of the type of the available excitation source.

Platinum/carbon multilayer reflectors for soft-x-ray optics.

We have fabricated platinum/carbon (Pt/C) multilayer reflectors with 2d spacaings between 50 and 200 Å, using an electron-beam evaporator. We investigated the effects of 2d values, the number of layer pairs, substrate temperature, coatings, and the long-term stability on the reflectivity performance by using characteristic x rays and monochromatized synchrotron radiation in the 0.8-8-keV region. In this study we show that Pt/C multilayers with 10-20 layer pairs exhibit high and stable soft-x-ray reflectivity. The interfacial roughness was measured in the range of 5 Å and becomes lower for structures deposited at liquid-nitrogen temperatures. Coating these reflectors with a 100-Å-thick platinum layer increased the grazing angle reflectivity without significantly lowering the Bragg peak reflectivity.