Ion Beam Analysis Techniques Research Articles

Andromede project: Surface analysis and modification with probes from hydrogen to nano-particles in the MeV energy range

The Andromede project is the center of a multi-disciplinary team which will build a new instrument for surface modification and analysis using the impact of probes from hydrogen to nano-particles (Au400+4) in the MeV range. For this new instrument a series of atomic, polyatomic, molecular and nano-particle ion beams will be delivered using two ion sources in tandem, a liquid metal ion source and an electron cyclotron resonance source. The delivered ion beams will be accelerated to high energy with a 4MeV van de Graaff type accelerator. By using a suite of probes in the MeV energy range, ion beam analysis techniques, MeV atomic and cluster secondary ion mass spectrometry can all be performed in one location. A key feature of the instrument is its ability to produce an intense beam for injection into the accelerator. The commissioning of the two sources shows that intense beams from atomic ions to nano-particles can be delivered for subsequent acceleration. The calculations and measurements for the two sources are presented.

Ion beam analysis of Cu(In,Ga)Se2 thin film solar cells

The present work investigates the potential of ion beam analysis (IBA) techniques such as the Rutherford backscattering spectrometry (RBS) and particle induced X-ray emission (PIXE) using helium ions to provide quantitative in-depth elemental analysis of various types of Cu(In,Ga)Se2 thin films. These films with a thickness of about 2μm are used as absorber layers in photovoltaic devices with continuously increasing the performance of this technology. The preparation process generally aims to obtain an in-depth gradient of In and Ga concentrations that optimizes the optoelectronic and electrical properties of the solar cell. The measurements were performed at directly accessible single or double layered CIGS absorbers and at buried absorbers in completed thin film solar cells. The IBA data were analyzed simultaneously in order to derive best fitted profiles that match all experimental RBS and PIXE spectra. For some samples elemental profiles deduced form synchrotron based, reference free grazing incidence X-ray fluorescence analysis were compared with the IBA results and an overall good agreement was observed within quoted uncertainties.

Gold layers characterization by Ion Beam Analytical Techniques: from Semiconductors to cultural heritage artefacts

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Use of proton elastic scattering techniques to determine carbonaceous fractions in atmospheric aerosols collected on Teflon filters

Amongst Ion Beam Analysis (IBA) techniques applied to the study of atmospheric aerosol samples, Elastic Backscattering Spectrometry (EBS) and Particle Elastic Scattering Analysis (PESA) with MeV energy proton beams allows obtaining quantitative information about the concentration of C and other low-Z atoms like H, N and O in the sample.With these nuclear techniques a direct measurement of elemental carbon (EC) and organic carbon (EC) is not possible. Nevertheless, the detection of all the aforemetioned light elements may help to infer some information on the aerosol chemical composition. The H concentration obtained by PESA may be used as a proxy of OC; then, EC can be obtained as the difference between total carbon measured simultaneously by EBS and OC as estimated by PESA. The feasibility of the quantification of EC and OC following this approach in particulate matter samples collected on Teflon filters, where this information cannot be obtained by standard thermo-optical analyses, will be discussed.Moreover, thanks to the simultaneous measurements of H, C, N and O in the aerosol samples, the organic component of the aerosols (particulate organic matter, POM) can be directly calculated and thus the validity of the POM/OC conversion factors found in the literature can be tested.

A new ion beam facility based on a 3 MV Tandetron™ at IFIN-HH, Romania

A 3MV Tandetron™ accelerator system has been installed and commissioned at the “Horia Hulubei” National Institute for Physics and Nuclear Engineering – IFIN-HH, Măgurele, Romania. The main purpose of this machine is to strengthen applied nuclear physics research ongoing in our institute for more than four decades. The accelerator system was developed by High Voltage Engineering Europa B.V. (HVE) and comprises three high energy beam lines. The first beam line is dedicated to ion beam analysis (IBA) techniques: Rutherford Backscattering Spectrometry – RBS, Nuclear Reaction Analysis – NRA, Particle Induced X-ray and γ-ray Emission – PIXE and PIGE and micro-beam experiments – μ-PIXE. The second beam line is dedicated to high energy ion implantation experiments and the third beam line was designed mainly for nuclear cross-sections measurements used in nuclear astrophysics. A unique feature, the first time in operation at an accelerator facility is the Na charge exchange canal (CEC), which is used to obtain high intensity beams of He− of at least 3μA. The results of the acceptance tests demonstrate the huge potential of this new facility in various fields, from IBA to radiation hardness studies and from medical or environmental applications to astrophysics. The main features of the accelerator are presented in this paper.

Large areas elemental mapping by ion beam analysis techniques

The external beam line of the Laboratory for Material Analysis with Ion Beams (LAMFI) is a versatile setup for multi-technique analysis. X-ray detectors for Particle Induced X-rays Emission (PIXE) measurements, a Gamma-ray detector for Particle Induced Gamma- ray Emission (PIGE), and a particle detector for scattering analysis, such as Rutherford Backscattering Spectrometry (RBS), were already installed. In this work, we present some results, using a large (60-cm range) XYZ computer controlled sample positioning system, completely developed and build in our laboratory. The XYZ stage was installed at the external beam line and its high spacial resolution (better than 5 μm over the full range) enables positioning the sample with high accuracy and high reproducibility. The combination of a sub-millimeter beam with the large range XYZ robotic stage is being used to produce elemental maps of large areas in samples like paintings, ceramics, stones, fossils, and all sort of samples. Due to its particular characteristics, this is a unique device in the sense of multi-technique analysis of large areas. With the continuous development of the external beam line at LAMFI, coupled to the robotic XYZ stage, it is becoming a robust and reliable option for regular analysis of trace elements (Z > 5) competing with the traditional in-vacuum ion-beam-analysis with the advantage of automatic rastering.

Hybrid nanostructured thin-films by PLD for enhanced field emission performance for radiation micro-nano dosimetry applications

We report the observation of hybrid nanostructured thin-films such as diamond-like carbon (DLC) signature on the ZnO epitaxial thin-films grown onto the device silicon/quartz substrate by reactive pulsed laser deposition (r-PLD) under the argon–oxygen (Ar|O2) ambient at 573 K. Undoped and Carbon (C) doped epitaxial ZnO thin-film layer formation is revealed by the accelerator based ion-beam analysis (IBA) technique of resonant Rutherford backscattering spectrometry (RRBS), glancing-incidence X-ray diffraction (GIXRD) pattern, micro-Raman spectroscopy (μ-RS) and field-emission (F-E) studies. The RRBS and GIXRD results show the deposition of epitaxial thin-films containing C into ZnO. The μ-RS technique is a standard nondestructive tool (NDT) for the characterization of crystalline, nano-crystalline, and amorphous carbons (a-C). As grown ZnO and C-doped ZnO thin-films μ-RS result reveal the doping effect of C-impurities that appear in the form of DLC evident from Raman peaks at 1357 and 1575 cm−1 along with a wurtzite structure peak at 438 cm−1 with E2(h) phonon of ZnO. The electron transport F-E result shows the hybrid thin-films has high conductivity than the un-doped film. Fabricated hybrid nanostructured thin-films materials could be very useful for the emerging applications of micro-nano dosimetry.

Determination of the density of silicon–nitride thin films by ion-beam analytical techniques (RBS, PIXE, STIM)

This work presents the investigation of some commercially available and commonly used Si3N4 foils prepared with LPCVD technique. The density and the stoichiometry of these films were determined by Rutherford backscattering spectroscopy and profilometry, while the study of impurities was achieved with particle induced X-ray emission method. It was found that the density of the studied Si3N4 films is significantly less (~2.71 g cm−3), while the stoichiometry is close to the values of the bulk material. The results were verified by measuring the ion energy loss through the films by scanning transmission ion microscopy.

µ-XRF Analysis of Trace Elements in Lapis Lazuli-Forming Minerals for a Provenance Study.

This paper presents new developments on the provenance study of lapis lazuli started by our group in 2008: during the years a multi-technique approach has been exploited to obtain minero-petrographic characterization and creation of a database considering only rock samples of known provenance. Since the final aim of the study is to develop a method to analyze archeological findings and artworks made with lapis lazuli in a completely non-invasive way, ion beam analysis techniques were employed to trace the provenance of the raw material used for the production of artifacts. Continuing this goal and focusing the analysis on determination of more significant minero-chemical markers for the provenance study of trace elements in different minerals, the method was extended with the use of micro X-ray fluorescence (µ-XRF), to test the potential of the technique for this application. The analyzes were focused on diopside and pyrite in lapis lazuli samples of known provenance (Afghanistan, Tajikistan, and Siberia). In addition, µ-XRF data were compared with micro proton-induced X-ray emission (µ-PIXE) results to verify the agreement between the two databases and to compare the analytical performance of both techniques for this application.

Calibration of a new experimental chamber for PIXE analysis at the Accelerator Facilities Division of Atomic Energy Centre Dhaka (AECD)

A new experimental chamber has been installed at the 3MV Van de Graaff Accelerator Facilities Division in the Atomic Energy Centre, Dhaka, to perform different Ion Beam Analysis (IBA) techniques. The calibration of this new setup for Particle Induced X-ray Emission (PIXE) technique has been done using a set of thin MicroMatter standards and GUPIX (PIXE spectrum analysis software), which is explicated in this paper. The effective thicknesses of the beryllium window of the X-ray detector and of the different absorbers used were determined. For standardization, the so called instrumental constant H (product of detector solid angle and the correction factor for the setup) as function of X-ray energy were determined and stored inside the GUPIX library for further PIXE analysis.

Fuel retention in JET ITER-Like Wall from post-mortem analysis

Selected Ion Beam Analysis techniques applicable for detecting deuterium and heavier impurities have been used in the post-mortem analyses of tiles removed after the first JET ITER-Like Wall (JET-ILW) campaign. Over half of the retained fuel was measured in the divertor region. The highest figures for fuel retention were obtained from regions with the thickest deposited layers, i.e. in the inner divertor on top of tile 1 and on the High Field Gap Closure tile, which resides deep in the plasma scrape-off layer. Least retention was found in the main chamber high erosion regions, i.e. in the mid-plane of Inner Wall Guard Limiter. The fuel retention values found typically varied with deposition layer thicknesses. The reported retention values support the observed decrease in fuel retention obtained with gas balance experiments of JET-ILW.

Study of tungsten based positron moderators

Positrons and how they interact with matter has a growing interest in many fields. Most of their uses require the production of slow positron beams with a well-defined energy, but since these particles are usually generated by means of a radioactive source, they are fast and with a broad distribution of energies. For this reason it is necessary to moderate them to lower energies via inelastic collisions. Then, they can be accelerated to the desired energies. This requires the use of a moderator. Tungsten is one of the most commonly used moderator materials because of its reasonable efficiency and relatively low cost. In this work we present different methods of producing transmission tungsten-based moderators, with particular interest in a combination of tungsten thin foils and grids. We also show results about the characterization of these moderators by ion beam analysis and microscopy techniques along with their relative moderation efficiencies.

Assessment of dye distribution in sensitized solar cells by microprobe techniques

Dye sensitized solar cells (DSCs) have received considerable attention once this technology offers economic and environmental advantages over conventional photovoltaic (PV) devices. The PV performance of a DSC relies on the characteristics of its photoanode, which typically consists of a nanocrystalline porous TiO2 film, enabled with a large adsorptive surface area. Dye molecules that capture photons from light during device operation are attached to the film nanoparticles. The effective loading of the dye in the TiO2 electrode is of paramount relevance for controlling and optimizing solar cell parameters. Relatively few methods are known today for quantitative evaluation of the total dye adsorbed on the film. In this context, microprobe techniques come out as suitable tools to evaluate the dye surface distribution and depth profile in sensitized films. Electron Probe Microanalysis (EPMA) and Ion Beam Analytical (IBA) techniques using a micro-ion beam were used to quantify and to study the distribution of the Ru organometallic dye in TiO2 films, making use of the different penetration depth and beam sizes of each technique. Different 1D nanostructured TiO2 films were prepared, morphologically characterized by SEM, sensitized and analyzed by the referred techniques. Dye load evaluation in different TiO2 films by three different techniques (PIXE, RBS and EPMA/WDS) provided similar results of Ru/Ti mass fraction ratio. Moreover, it was possible to assess dye surface distribution and its depth profile, by means of Ru signal, and to visualize the dye distribution in sample cross-section through X-ray mapping by EPMA/EDS. PIXE maps of Ru and Ti indicated an homogeneous surface distribution. The assessment of Ru depth profile by RBS showed that some films have homogeneous Ru depth distribution while others present different Ru concentration in the top layer (2μm thickness). These results are consistent with the EPMA/EDS maps obtained.

Retention and thermal release behavior of deuterium and helium implanted in SiC

Retention and release of ion implanted deuterium (D) and helium (He) in silicon carbide (SiC) were studied with respect to damage accumulation and annealing behavior using ion beam analysis techniques. α-SiC single crystals were irradiated by 10keV D2+ and He+ at 300 and 770K, and depth profiles of retained atoms and lattice disorder were measured during the implantation and successive heat treatments. For the sample pre-irradiated with He at a fluence of 1.0×1021ions/m2, the thermal release of D atoms was completed at an annealing temperature of 1370K, while the retained D atoms still remained in the sample without pre-irradiation. In contrast to the facilitated thermal release of D by He pre-irradiation, the He release temperature increased in the sample followed by D ion implantation. No significant difference of He retention and damage accumulation behavior was observed between the samples implanted at 300 and 770K. The D retention and D-ion-induced disorder for 770K implantation, was reduced to approximately 1/2 comparing to that of the sample implanted at 300K. The D retention at 770K was not affected by the He pre-implantation induced damage.

Comparison between XRF and IBA techniques in analysis of fine aerosols collected in Rijeka, Croatia

The new system for energy dispersive X-ray fluorescence (EDXRF) analysis has been installed at the Laboratory for Elemental Micro-Analysis (LEMA) at the University of Rijeka. Currently the key application of this new XRF system is in the field of environmental science, i.e.in the analysis of fine airborne particles. In this work, results of initial multi-elemental analysis of PM2.5 fraction is reported for the first time in the region of Rijeka, Croatia. Sampling was performed at the Rijeka City center, during a continuous 9-day period in February/March 2012. All samples were collected on stretched Teflon filters in 12h periods. To check the reliability of the new XRF system, results of XRF analysis are compared with the results obtained by the well-established Ion Beam Analysis (IBA) laboratory at Australian Nuclear Science and Technology Organisation (ANSTO). The concentrations of H, Na, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Br and Pb were determined. In addition, black carbon was determined by Laser Integrating Plate Method (LIPM). Very good agreement between XRF and IBA techniques is obtained for all elements detected by both techniques. Elemental concentrations were correlated with the traffic volume and wind speed and direction. The summary of our findings is presented and discussed in this paper.

Development of a PIXE method at high energy with the ARRONAX cyclotron

The high energy PIXE (HEPIXE) method is a multi-elemental non-destructive ion beam analysis technique. It is based on the detection of the X-ray emitted due to the interaction of high energy particle beam with a sample. This technique is fast and allows the analysis of heavy and medium elements in thin (lm), thick (mm) and multilayer samples. At the ARRONAX facility (Nantes, France), the HEPIXE method has been used to determine the composition of natural and synthetic sodalites. Photochromic properties of these samples are supposed to come from the trace elements (concentration in the ppm range) present in the samples. Taking advantage of the 70 MeV proton beam available at our facility, the HEPIXE method has been also used to study multilayer samples. It has been shown that it is possible to determine the composition of each layer, their thicknesses and their depth position by analyzing the recorded X-ray spectra.

Single cell in situ detection and quantification of metal oxide nanoparticles using multimodal correlative microscopy.

Assessing in situ nanoparticles (NPs) internalization at the level of a single cell is a difficult but critical task due to their potential use in nanomedicine. One of the main actual challenges is to control the number of internalized NPs per cell. To in situ detect, track, and above all quantify NPs in a single cell, we propose an approach based on a multimodal correlative microscopy (MCM), via the complementarity of three imaging techniques: fluorescence microscopy (FM), scanning electron microscopy (SEM), and ion beam analysis (IBA). This MCM was performed on single targeted individual primary human foreskin keratinocytes (PHFK) cells cultured and maintained on a specifically designed sample holder, to probe either dye-modified or bare NPs. The data obtained by both FM and IBA on dye-modified NPs were strongly correlated in terms of detection, tracking, and colocalization of fluorescence and metal detection. IBA techniques should therefore open a new field concerning specific studies on bare NPs and their toxicological impact on cells. Complementarity of SEM and IBA analyses provides surface (SEM) and in depth (IBA) information on the cell morphology as well as on the exact localization of the NPs. Finally, IBA not only provides in a single cell the in situ quantification of exogenous elements (NPs) but also that all the other endogenous elements and the subsequent variation of their homeostasis. This unique feature opens further insights in dose-dependent response analyses and adds the perspective of a better understanding of NPs behavior in biological specimens for toxicology or nanomedicine purposes.

Elemental compositions of PM10–2.5 and PM2.5 aerosols of a Nigerian urban city using ion beam analytical techniques

The paucity of data on air quality studies in Nigeria prompted us to commence the sampling of particulate matter (PM10–2.5 and PM2.5) in Mushin Lagos, Nigeria. Both size-segregated fractions were collected using a double staged ‘Gent’ stack filter unit sampler. Elemental characterization was carried out by Particle Induced X-ray Emission (PIXE) and Proton Induced γ-ray Emission (PIGE) techniques using an external ion beam set-up. Twenty-four elements (Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Se, Br, Rb, Sr, Zr, Cs and Pb) were detected in both fractions and their concentrations were assessed. A study of their inter-elemental correlations indicated that some elements could have common source origins or similar chemical properties while enrichment factors (EF) displayed that most elements emanated from anthropogenic sources. Source apportionment studies are thus recommended.

Rutherford forward scattering and elastic recoil detection (RFSERD) as a method for characterizing ultra-thin films

We present a novel ion beam analysis technique combining Rutherford forward scattering and elastic recoil detection (RFSERD) and demonstrate its ability to increase efficiency in determining stoichiometry in ultrathin (5–50nm) films as compared to Rutherford backscattering. In the conventional forward geometries, scattering from the substrate overwhelms the signal from light atoms but in RFSERD, scattered ions from the substrate are ranged out while forward scattered ions and recoiled atoms from the thin film are simultaneously detected in a single detector. The technique is applied to tantalum oxide memristors but can be extended to a wide range of materials systems.

Surface analysis of tiles and samples exposed to the first JET campaigns with the ITER-like wall

This paper reports on the first post-mortem analyses of tiles removed from JET after the first campaigns with the ITER-like wall (ILW) during 2011–12 []. Tiles from the divertor have been analysed by ion beam analysis techniques and by secondary ion mass spectrometry to determine the amount of beryllium deposition and deuterium retention in the tiles exposed to the scrape-off layer. Films 10–20 μm thick were present at the top of tile 1, but only very thin films (< 1 μm) were found in the shadowed areas and on other divertor tiles. The total amount of Be found in the divertor following the ILW campaign was a factor of ∼ 9 less than the material deposited in the 2007–09 carbon campaign, after allowing for the longer operations in 2007–09.