Depth Distribution Of Elements Research Articles

Effect of titanium ion implantation and deposition on hydrogenation behavior of Zr-1Nb alloy

In order to study the effect of titanium ion implantation and deposition on hydrogenation behavior of Zr–1Nb alloy, the samples were subjected to plasma immersion implantation and deposition (PIII&D) of titanium ions at the bias voltage of 0.5–1.5kV using a filtered metal vapor vacuum arc source. The crystalline structure, surface morphology and depth distributions of elements in the surface layer of the samples were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and glow-discharge optical emission spectroscopy (GD-OES), respectively. Hydrogen saturation was performed from hydrogen atmosphere at 673K temperature and 2atm. pressure. It was found that hydrogen absorption rate by Zr–1Nb alloy decreased after PIII&D. The modified layers contained a mixing zone of titanium and zirconium, which decreases with increasing bias voltage. Hydrogenation causes the formation of titanium hydrides and lattice distortions of α–Zr at the low bias voltage that does not occur at higher bias voltages. The hydrogenation behavior of modified zirconium alloy was discussed.

Quantitative spectromicroscopy from inelastically scattered photoelectrons in the hard X-ray range

We demonstrate quantitative, highly bulk-sensitive x-ray photoelectron emission microscopy by analysis of inelastically scattered photoelectrons in the hard X-ray range, enabling elemental depth distribution analysis in deeply buried layers. We show results on patterned structures used in electrical testing of high electron mobility power transistor devices with an epitaxial Al0.25Ga0.75N channel and a Ti/Al metal contact. From the image series taken over an energy range of up to 120 eV in the Ti 1s loss feature region and over a typical 100 μm field of view, one can accurately retrieve, using background analysis together with an optimized scattering cross-section, the Ti depth distribution from 14 nm up to 25 nm below the surface. The method paves the way to multi-elemental, bulk-sensitive 3D imaging and investigation of phenomena at deeply buried interfaces and microscopic scales by photoemission.

Influence of plasma immersion titanium implantation on hydrogenation and mechanical properties of Zr–2.5Nb

This paper describes the effect of plasma immersion ion implantation (PIII) of titanium on hydrogenation behavior and mechanical properties of Zr–2.5Nb alloy. Surface morphology and depth distribution of elements in the surface layer of the samples were analyzed by scanning electron (SEM) and atomic force microscopy (AFM), and glow-discharge optical emission spectroscopy (GDOES). Hydrogenation was performed at 673K temperature and 2atm pressure. It was found that after titanium implantation a diffusion barrier is formed, accumulating hydrogen and preventing hydrogen penetration in the sample volume. The microdroplet content significantly influences the hydrogenation behavior of the zirconium alloy. Hydrogen sorption rate decreased 18.3 times and 4.3 times using filtered and unfiltered PIII, respectively. The mechanical properties of titanium-implanted zirconium layer were improved. The degradation of the mechanical properties after hydrogenation was revealed.

Hydrogenation of Zr-2.5Nb alloy after plasma-immersion titanium implantation

The study results of the influence of plasma-immersion ion implantation of titanium in Zr-2.5Nb on hydrogenation are presented. The titanium implantation was carried out in two modes: with active plasma filtering (APF) and passive plasma filtering (PPF). The results of total hydrogen concentration, absorption rate, XRD analyses and depth distribution of elements revealed that modified surface layer after titanium ion implantation is formed hydrogen diffusion barrier reduces hydrogen absorption by Zr-2.5Nb.

Multi-functional TiO2/Si/Ag(Cr)/TiNx coatings for low-emissivity and hydrophilic applications

Multi-functional (coatings with some additional functional properties such as high transparency, antireflection, hydrophilicity and antifogging) coatings are indispensable for the modern energy saving systems. In this regard, we deposited TiO2/Si/Ag(Cr)/TiNx multilayer thin films on soda-lime glass by using RF and DC magnetron sputtering to achieve a multi-functional thin film stack with the combination low-emissivity (low-e) and hydrophilicity properties in addition to the high transparency. Primary deposition of Ag(Cr)/TiNx was tried for the low-e effect and successfully obtained a very low emissivity value of 0.067, and then Si and TiO2 films with different bandgap were subsequently deposited to provide the hydrophilic properties. X-ray diffraction results revealed the anatase phase formation of TiO2 after annealing the films at 673K by using the rapid thermal annealing system. Rutherford Backscattering Spectrometry (RBS) was carried out to determine the chemical composition and elemental depth distribution. The multilayer stack exhibited superhydrophilicity with a water contact angle of about 5° after irradiation by UV light. A Heterojunction film with wide and narrow bandgap semiconductor materials was effective to improve the hydrophilicity. The films exhibited a high visible transmittance (∼85.5%, at 550nm) and low infrared transmittance (7%, at 2000nm) including low-e and superhydrophilicity.

Study of annealing-induced interdiffusion in In2O3/Ag/In2O3 structures by a combined X-ray reflectivity and grazing incidence X-ray fluorescence analysis

The combination of X-ray reflectivity and grazing incidence X-ray fluorescence has been applied to the characterization of an In2O3/Ag/In2O3 stack for advanced photovoltaic applications. X-ray reflectivity is a well-known method for the characterization of multilayered structures by providing information on the thickness and the in-depth electronic density. Grazing incidence X-ray fluorescence provides information about the elemental depth distribution. As these techniques are based on similar measurement procedures and data evaluation approaches, their combination reduces the uncertainties of the individual techniques and provides an accurate depth-resolving analysis of multi-layers.It has been shown that the combination of the techniques give insight into the material composition and the layers structure (thickness, density) as well as modifications induced by a thermal annealing.As X-ray fluorescence signals have been acquired at different excitation energies, the influence of this parameter on the sensitivity of the measurements to the structural properties has been shown.

Passivation behaviour of 304 stainless steel in an ionic liquid with a fluorinated anion

The effect of immersion of type 304 stainless steel in pyrrolidium-2-one trifluoroacetate ionic liquid on surface composition and structure was studied. A passive film with increased protective properties was formed on the steel surface due to enrichment of chromium in the inner region of the oxide film and enrichment of nickel beneath the oxide film. The presence of fluorine bonded to metal and carbon was revealed on the surface of steel that was attributed to interaction of the steel and anions of the ionic liquid. Newly developed plasma profiling time-of-flight mass spectrometry was successfully employed for semi-quantitative analysis of the elemental depth distributions in the thin passive film with high resolution.

Several approaches to the investigation of paintings with the use of portable X-ray fluorescence analysis

Abstract This paper deals with several approaches to the application of X-ray fluorescence analysis and micro-analysis to non-destructive investigations of paintings. The methodology is described and demonstrated on a painting of known structure that was painted with modern artistic tempera paints. There is also a description and a demonstration of three depth profiling techniques that provide information on the depth distribution of elements in the surface layers of a painting. The three techniques utilize (a) the internal X-ray ratios of the elements that are present, (b) X-ray fluorescence analysis with two detectors with different angles of detection of characteristic X-rays, and (c) a technique based on comparing X-ray spectra measured with a tilted sample. The capabilities and demands on instrumentation and interpretation of the results are compared for all these techniques.

Influence of Surface Roughness on Interdiffusion Processes in InGaP/Ge Heteroepitaxial Thin Films

In the present work, we report on the study of InGaP/Ge heterojunctions grown by metal organic vapor phase epitaxy at different growth temperatures, with the aim of analyzing properties of the layer and interface between InGaP epilayer and germanium substrate. Secondary Neutral Mass Spectroscopy, Rutherford Backscattering Spectrometry, High Resolution X-Ray Diffraction, Transmission Electron Microscopy and Atomic Force Microscopy have been used to characterize the layers. The main goal of this work is to get information about diffusion processes of Ga, In, P in the substrate and of Ge in the epitaxial film. Since the interface roughness during sputtering and the effect of diffusion depends on the growth temperature, depth profiles measured experimentally were combined with surface roughness data in order to get more reliable information about diffusion profiles and the real depth distribution of elements in the interface.

Analysis of lustred ceramics of the Galleria Regionale di Palazzo Bellomo di Siracusa, Italy

Several fragments of lustred pottery coming from the collection of the Galleria Regionale di Palazzo Bellomo and excavated in Siracusa, were studied through non-invasive ion beam techniques in the Centre de Recherche et de Restauration des Musees de France in Paris. Up to now only aesthetic and stylistic analysis were available for these objects, and their provenances and dating were unknown or uncertain; moreover, the question concerning a possible local production was still debated. Compositions of pottery and glazed parts were thus obtained by Particle Induced X-ray Emission analysis, while the depth distribution of element of the lustre was analyzed by the Rutherford Backscattering Spectrometry technique. The obtained results provided important information on possible origin and production period of the objects.

Development of a low-energy PIXE analysis system based on an ion implanter

A low-energy particle-induced X-ray emission (LE-PIXE) analysis system with precise energy control was developed based on a 200kV ion implanter. The energy dependence of LE-PIXE was evaluated using a millimeter-sized low-energy proton beam by varying the incident energy with precision better than 5keV. LE-PIXE spectra were obtained for protons with an energy range of 40–120keV. The LE-PIXE sensitivity was approximately proportional to the sixth power of the incident proton energy. The characteristic X-ray intensity strongly depended on the depth distribution of elements in the target. Experimental evaluation with multilayered thin film samples demonstrated that LE-PIXE was effective for depth distribution analysis to 1000nm deep. Multilayered structures containing four different elements were characterized by LE-PIXE analysis using multiple probe energies.

Characterization of Li deposition on the first wall of EAST using laser-induced breakdown spectroscopy

Our recent investigations have indicated that laser-induced breakdown spectroscopy (LIBS) may have great potential in the monitoring of the deposition features of plasma-facing materials (PFMs) in experimental advanced superconducting tokamak (EAST). Detailed information on these PFM can be obtained in real time by analyzing the spectra from 200 to 980 nm. The depth distribution of the main elements from PFMs of the EAST divertor was here investigated. The decrease in the concentrations of main deposed elements (such as Li, Fe, and Cr) were clearly observable after the first ten laser pulses at a laser power density of 5 × 109 W/cm2. The concentrations of substrate elements were found to be uniformly distributed along the depth axis. The use of LIBS for the characterization of quasi three-dimensional multielement distribution maps of the deposition of impurities in the gaps between divertor tiles is here presented. This significantly improves the understanding of the Li deposition behavior of EAST.

Depth‐selective elemental imaging of microSD card by confocal micro XRF analysis

A semiconductor device, a microSD card, was measured by using two XRF instruments. 2D elemental images were obtained using a micro‐XRF system with a spatial resolution of 10 µm. Elemental distributions of the near‐surface region of the sample were clearly shown. Titanium was observed in the resin constituting the sample. Nickel and gold were observed on a terminal and localization of the sample. Elemental distribution of copper reflected the circuit structure of the measurement area that was in the neighborhood of the sample surface. Moreover, the elemental depth distributions of the sample were measured by using a confocal micro‐XRF instrument. The confocal micro‐XRF instrument was constructed in the laboratory with fine‐focus polycapillary x‐ray optics. The depth resolution of the developed spectrometer was 13.7 µm at an energy of Au Lβ (11.4 keV). The elemental images obtained at near‐surface by confocal micro‐XRF were the same as the results obtained from 2D micro‐XRF. However, different Cu images were obtained at a depth of several tens of micrometers. This indicates that microSD cards consist of a few different Cu‐circuit structure designs. The elemental depth distributions of each circuit structure of the semiconductor device were clearly shown by confocal micro‐XRF. Copyright © 2013 John Wiley & Sons, Ltd.

Comparison of SEM-EDS, Micro-XRF and Confocal Micro-XRF for Electric Device Analysis

In general, scanning electron microscope with energy dispersive X-ray spectroscopy (SEM-EDS) has been used in laboratories or factories for the analysis of the element distribution in the samples such as electric components. However, SEM-EDS requires sample preparation, which usually is difficult and takes a long time. On the other hand, micro X-ray fluorescence (μ-XRF) can be utilized for the elemental analysis underneath the surface of the samples thanks to the high penetrating power of X-rays. Furthermore, the depth distribution of elements in the samples can be acquired by the latest confocal XRF. In this paper, the information regarding the depth direction in small electrical and electronic components is compared for SEM-EDS, μ-XRF and the confocal XRF. At the same time, we give a brief report on not only the development of confocal XRF equipment but also some ideas as to the depth profile of the samples. [DOI: 10.1380/ejssnt.2013.133]

Effect of the Deposition Time onto Structural Properties of Cu2ZnSnS4 Thin Films Deposited by Pulsed Laser Deposition

The <TEX>$Cu_2ZnSnS_4$</TEX> (CZTS) thin film solar cell is a candidate next generation thin film solar cell. For the application of an absorption layer in solar cells, CZTS thin films were deposited by pulsed laser deposition (PLD) at substrate temperature of <TEX>$300^{\circ}C$</TEX> without post annealing process. Deposition time was carefully adjusted as the main experimental variable. Regardless of deposition time, single phase CZTS thin films are obtained with no existence of secondary phases. Irregularly-shaped grains are densely formed on the surface of CZTS thin films. With increasing deposition time, the grain size increases and the thickness of the CZTS thin films increases from 0.16 to <TEX>$1{\mu}m$</TEX>. The variation of the surface morphology and thickness of the CZTS thin films depends on the deposition time. The stoichiometry of all CZTS thin films shows a Cu-rich and S-poor state. Sn content gradually increases as deposition time increases. Secondary ion mass spectrometry was carried out to evaluate the elemental depth distribution in CZTS thin films. The optimal deposition time to grow CZTS thin films is 150 min. In this study, we show the effect of deposition time on the structural properties of CZTS thin film deposited on soda lime glass (SLG) substrate using PLD. We present a comprehensive evaluation of CZTS thin films.

Synchrotron radiation based micro X-ray fluorescence analysis of the calibration samples used in surface sensitive total reflection and grazing emission X-ray fluorescence techniques

Total reflection X-ray fluorescence (TXRF) and grazing emission X-ray fluorescence (GEXRF) are surface sensitive techniques and can be used for detailed surface studies of different materials, including ultra-low concentration contamination or the lateral and depth distributions of elements. The calibration procedure typically used involves placing a micro-droplet (∼μl) of the standard solution onto a silicon wafer (or quartz backing). After evaporation of the solvent, the residual amount of elements is used as a reference standard. Knowledge of the distribution of residue material on the substrate surface is crucial for precise quantification. In the present work the investigation of the lateral distribution of elements in the multielemental calibrating samples, containing the 23 most commonly studied elements, by using the synchrotron radiation based micro X-ray fluorescence is presented. The goal of this project was the study of a uniformity of the elemental distributions and determination of the residual elements morphology depending on the temperature of the drying process. The X-ray images were compared with optical and SEM images. Paper presents in details the experimental setup, sample preparation procedures, measurements and results. In the analysis of the X-ray images of the sample dried in high temperature the censoring approach was applied improving the quality of statistical analysis. The information on the elements distribution in the calibrating samples can be useful for developing more accurate calibration procedures applied in quantitative analysis of surface sensitive TXRF and GEXRF techniques.

Tribology behavior of double-glow discharge Mo layers on titanium alloy in aviation kerosene environment

In order to improve the tribology behavior in aviation kerosene, molybdenum (Mo) modified layers were fabricated on Ti6Al4V base alloy using a double-glow plasma surface alloying technique. The morphology, microstructure, microhardness and element depth distribution of the Mo modified layers were studied. The tribology properties of Ti6Al4V base alloy, Mo modified layers and 5CrMnMo tool steel sliding with GCr15 steel or QSn4-3 copper alloy counterparts in aviation kerosene were comparatively researched. The effect of roughness on the sliding wear behavior was discussed. The results indicate that the Mo modified layers with polishing treatments not only reduce the friction coefficient of Ti6Al4V base, but also enhance the wear resistance of the counterparts. The Mo modified layers have better tribology behavior than 5CrMnMo steel. It is also found that the wear volume loss of the counterparts is proportional to the value of roughness of Mo modified layers, which is related directly to the ploughing wear between micro convex bodies of the layers and counterparts.

Inhomogeneous nanostructured honeycomb optical media for enhanced cathodo- and under-x-ray luminescence

Photo-, radio-, and pulse cathodoluminescence spectra from sol-gel derived titania, doped with strontium and terbium, deposited on porous anodic alumina (PAA) films are reported. The morphology and qualitative elemental depth distributions have been examined by transmission electron microscopy, scanning electron microscopy, and radio-frequency glow discharge optical emission spectroscopy. PAA films with pore and cell sizes ranging from 170 to 190 and 240 to 270 nm, respectively, have been generated on aluminum and monocrystalline silicon substrates followed by spin-on sol-gel derived coating with the subsequent thermal treatment. The resultant PAA surface is not coated with a continuous xerogel film; the xerogel is mainly distributed near the pore bases, leaving much of the pore volume unfilled. The xerogel/PAA structures reveal terbium-related luminescence under x-ray excitation and cathodoluminescence. The same xerogels generated on monocrystalline silicon revealed no cathode- or under-x-ray luminescence. Thus, PAA enhances strongly the cathode- and under x-ray luminescence from terbium and strontium-doped titania xerogels confined in the porous matrix. The fabricated structures are considered as a type of low-cost, thin-film convertor of x-rays, and cathode ray irradiation into visible light, with an average cell size of the convertor of about 250 nm.

Compositional analysis and depth profiling of thin film CrO2 by heavy ion ERDA and standard RBS: a comparison

Chromium dioxide (CrO 2 ) thin film has generated considerable interest in applied research due to the wide variety of its technological applications. It has been extensively investigated in recent years, attracting the attention of researchers working on spintronic heterostructures and in the magnetic recording industry. However, its synthesis is usually a difficult task due to its metastable nature and various synthesis techniques are being investigated. In this work a polycrystalline thin film of CrO 2 was prepared by electron beam vaporization of Cr 2 O 3 onto a Si substrate. The polycrystalline structure was confirmed through XRD analysis. The stoichiometry and elemental depth distribution of the deposited film were measured by ion beam nuclear analytical techniques heavy ion elastic recoil detection analysis (ERDA) and Rutherford backscattering spectrometry (RBS), which both have relative advantage over non-nuclear spectrometries in that they can readily provide quantitative information about the concentration and distribution of different atomic species in a layer. Moreover, the analysis carried out highlights the importance of complementary usage of the two techniques to obtain a more complete description of elemental content and depth distribution in thin films. Heavy ion elastic recoil detection analysis (ERDA) and Rutherford backscattering spectrometry (RBS) both have relative advantage over non-nuclear spectrometries in that they can readily provide quantitative information about the concentration and distribution of different atomic species in a layer. ► Thin films of CrO 2 have been grown by e-beam evaporation of Cr 2 O 3 target in vacuum. ► The composition was determined by heavy ion—ERDA and RBS. ► HI-ERDA and RBS provided information on the light and heavy elements, respectively.

Publisher’s Note: “In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x ray fluorescence and diffraction” [J. Appl. Phys. 109, 123515 (2011)

Publisher’s Note: “<i>In situ</i> analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x ray fluorescence and diffraction” [J. Appl. Phys. 109, 123515 (2011)