Application Of Ion Beam Analysis Research Articles

Differential cross–section measurements for the proton-induced alpha and deuteron reactions and elastic scattering on 9Be, suitable for Ion beam analysis applications

In the current work the differential cross sections for the proton-induced 9Be(p,d0)8Be and 9Be(p,α0)6Li nuclear reactions (Q-values = 559 and 2125 keV respectively), as well as, the 9Be(p,p0)9Be elastic scattering were measured for 6 backscattering detection angles (θ = 120°, 130°, 140°, 150°, 160° and 170°) covering the Ep,lab = 300–3000 keV energy range with an energy step between 10 and 50 keV. The total estimated uncertainties of the determined cross-section values did not exceed 6.4 % for the elastic scattering, 7.0 % for the 9Be(p,α0)6Li and 9.9 % for the 9Be(p,d0)8Be reaction. Benchmarking measurements were also performed with a suitable thick target in order to validate the obtained cross-section values. The present experimental results constitute three coherent differential cross-section datasets suitable for IBA applications. The measurements were performed at the 4 MV Tandem Dynamitron Laboratory of the Ruhr University Bochum in Germany. The experimental, data analysis and benchmarking procedures are presented in detail.

Recent Achievements in NAA, PAA, XRF, IBA and AMS Applications for Cultural Heritage Investigations at Nuclear Physics Institute, Řež

Five case studies are reported on the use of neutron and photon activation analysis (NAA and PAA, respectively), X-ray fluorescence (XRF) analysis, ion beam analysis (IBA), and accelerator mass spectrometry (AMS) for the elemental characterization or dating of various objects of cultural heritage, such as building materials, pottery, metallic artefacts, ancient decorations, or the remains of historical personalities. The use of the individual techniques or their combination proved a useful, frequently indispensable tool for revealing the provenance of the artefacts, the method and time of their manufacturing, the elucidation of ancient human activities, or the verification of various hypotheses or legends related to the artefacts.

Quantitative Lithiation Depth Profiling in Silicon Containing Anodes Investigated by Ion Beam Analysis

The localisation and quantitative analysis of lithium (Li) in battery materials, components, and full cells are scientifically highly relevant, yet challenging tasks. The methodical developments of MeV ion beam analysis (IBA) presented here open up new possibilities for simultaneous elemental quantification and localisation of light and heavy elements in Li and other batteries. It describes the technical prerequisites and limitations of using IBA to analyse and solve current challenges with the example of Li-ion and solid-state battery-related research and development. Here, nuclear reaction analysis and Rutherford backscattering spectrometry can provide spatial resolutions down to 70 nm and 1% accuracy. To demonstrate the new insights to be gained by IBA, SiOx-containing graphite anodes are lithiated to six states-of-charge (SoC) between 0–50%. The quantitative Li depth profiling of the anodes shows a linear increase of the Li concentration with SoC and a match of injected and detected Li-ions. This unambiguously proofs the electrochemical activity of Si. Already at 50% SoC, we derive C/Li = 5.4 (< LiC6) when neglecting Si, proving a relevant uptake of Li by the 8 atom % Si (C/Si ≈ 9) in the anode with Li/Si ≤ 1.8 in this case. Extrapolations to full lithiation show a maximum of Li/Si = 1.04 ± 0.05. The analysis reveals all element concentrations are constant over the anode thickness of 44 µm, except for a ~6-µm-thick separator-side surface layer. Here, the Li and Si concentrations are a factor 1.23 higher compared to the bulk for all SoC, indicating preferential Li binding to SiOx. These insights are so far not accessible with conventional analysis methods and are a first important step towards in-depth knowledge of quantitative Li distributions on the component level and a further application of IBA in the battery community.

Application of Ion Beam Analysis in Studies of First Wall Materials in Controlled Fusion Devices

The paper provides a concise overview of ion beam analysis methods and procedures in studies of materials exposed to fusion plasmas in controlled fusion devices with magnetic confinement. An impact of erosion–deposition processes on the morphology of wall materials is presented. In particular, results for deuterium analyses are discussed. Underlying physics, advantages and limitations of methods are addressed. The role of wall diagnostics in studies of material migration and fuel retention is explained. A brief note on research and handling of radioactive and beryllium-contaminated materials is also given.

Application of ion beam analysis for the characterization of SiC- and DLC-thin films

Three series of protective coatings (thickness ca. 200-300 nm) were prepared on the surface of Ti-Al-V alloy (TA6V): silicon carbide (SiC) films produced by ion sputtering (I), silicon carbide films and subjected to Dynamic Ion Mixing (DIM) during the deposition procedure (II) and Diamond Like Carbon (DLC) films produced by ion beam deposition (III). The chemical composition (Si, C and O) of the films was determined using ion beam analysis techniques. The silicon, carbon and oxygen depth distribution was determined by proton Rutherford backscattering spectrometry (p-RBS) and using the resonances at 4.265 and 3.035 MeV of the 12C(α,α)12C and 16O(α,α)16O interactions respectively. The ratio of Si:C was found to be close to the stoichiometric one. The corrosion resistance of the coated samples was tested under strong aggressive conditions (5M HCl at 50 oC). The investigation following the corrosion attack showed that the thickness of the films remained practically unchanged. Only slight diffusion and dissolution effects were observed indicating the good quality of the produced thin films.

Characterization and application of automated in-vacuum PIXE/EBS system for direct analysis of chloride and sulfate ions attack in cementitious materials

Abstract Ion beam analysis (IBA) techniques (Particle Induced X-ray Emission, PIXE and Elastic Backscattering Spectrometry, EBS), were applied to investigate chloride and sulfate ions diffusion into laboratory prepared mortar samples. Development and characterization of an automated in-vacuum macro PIXE/EBS system is thoroughly discussed. Depth profile information of both chloride and sulfate ions in laboratory prepared mortar samples, after immersion in sea water for nine months, was rapidly and easily obtained at fairly low cost and with standardless analysis, demonstrating the value of the application of IBA to elemental depth profiling in cementitious materials. Chloride and sulfate depth profiles were obtained for two sets of mortar samples, one prepared with different water/cement (W/C) ratios and the other with different sand/cement (S/C) ratios. Results showed higher diffusion rates of both chloride and sulfate ions when both ratios are increased. Additionally, the W/C ratio has a stronger influence in both sulfate and chloride penetration than the S/C ratio, and chloride ions penetrate faster than sulfates. Advantages and limitations of applying IBA techniques in this investigation are discussed. The comparison between PIXE and other X-ray based analytical techniques, namely X-ray fluorescence (XRF) and energy and wavelength dispersive X-rays (EDX/WDX), as well as other traditional wet chemical methods is reviewed, and industrial applications are discussed.

System on chip (SoC) microcontrollers (μC) as digitisers for ion beam analysis (IBA) instruments

Data digitisation of the analogue signals from detectors to digital data is an essential process in ion beam analysis (IBA). The low-cost, easy availability and development environments that have a low learning threshold makes system-on-chip (SoC) microcontrollers (μC) attractive for this task. These μC combine, on one die, analogue and digital inputs and outputs with serial USB interfaces, which opens up simple implementation of tailor-made interfaces for specific IBA measurement systems. We have investigated the design and performance limitations based on development of three different digitisation interfaces for IBA. These were a two-channel nuclear instrumentation module (NIM) ADC event mode interface (EMI) for a high-resolution magnetic RBS spectrometer, a simple headless-multi-channel analyser (MCA) and a combined dual channel headless MCA and EMI. It is shown that SoC μC based interfaces for digitisation of analogue spectroscopy pulses in IBA systems can be implemented for material costs less than 100€. The performance of the SoC devices for many IBA applications is close to what can be achieved with state-of-the-art instruments. The simple pulse spectroscopy interface circuit and software are included in the auxiliary archive.

The role and application of ion beam analysis for studies of plasma-facing components in controlled fusion devices

First wall materials in controlled fusion devices undergo serious modification by several physical and chemical processes arising from plasma–wall interactions. Detailed information is required for the assessment of material lifetime and accumulation of hydrogen isotopes in wall materials. The intention of this work is to give a concise overview of key issues in the characterization of plasma-facing materials and components in tokamaks, especially in JET with an ITER-Like Wall. IBA techniques play a particularly prominent role here because of their isotope selectivity in the low-Z range (1–10), high sensitivity and combination of several methods in a single run. The role of 3He-based NRA, RBS (standard and micro-size beam) and HIERDA in fuel retention and material migration studies is presented. The use of tracer techniques with rare isotopes (e.g. 15N) or marker layers on wall diagnostic components is described. Special instrumentation, development of equipment to enhance research capabilities and issues in handling of contaminated materials are addressed.

The Application of Ion Beam Analysis to Mass Transport Studies in Mixed Electronic Ionic Conducting Electrodes

The measurement of the mass transport and oxygen exchange in materials for SOFCs has been greatly aided by the use of ion beam analysis techniques. In particular this has focused on the use of Secondary Ion Mass Spectrometry (SIMS) to measure diffusion profiles of oxygen 18 in ceramics to determine the kinetics of the bulk transport of oxygen. A second ion beam technique, Low Energy Ion Scattering (LEIS) can provide important information about the composition of the outermost atomic layers of the same materials where the gas/solid oxygen exchange process is taking place. The application of the newer technique of LEIS to materials for air electrodes is discussed and the behaviour of some common perovskite materials is explored.

Light and heavy ion beam analysis of thin biological sections

The application of ion beam analysis (IBA) techniques to thin biological sections (ThBS) presents unique challenges in sample preparation, data acquisition and analysis. These samples are often the end product of expensive, time-consuming experiments, which involve many steps that require careful attention. Analysis via several techniques can maximise the information that is collected from these samples. Particle-induced X-ray emission (PIXE) and Rutherford backscattering (RBS) spectroscopy are two generally non-destructive IBA techniques that use the same MeV ions and can be performed simultaneously. The use of heavy ion PIXE applied to thick samples has, in the past, resulted in X-ray spectra of a poorer quality when compared to those obtained with proton beams. One of the reasons for this is the shorter probing depth of the heavy ions, which does not affect thin sample analysis. Therefore, we have investigated and compared 3-MeV proton and 36-MeV carbon ion beams on 7-μm thick mouse brain sections at the ANSTO Heavy ion microprobe (HIMP). The application of a 36-MeV C4+ ion beam for PIXE mapping of ThBS on thin Si3N4 substrate windows produced spectra of high quality that displayed close to a nine-times gain in signal yield (Z2/q) when compared to those obtained for 3-MeV protons for P, S, Cl and K but not for Fe, Cu and Zn. Image quality was overall similar; however, some elements showed better contrast and features with protons whilst others showed improved contrast with a carbon ion beam. RBS spectra with high enough counting statistics were easily obtained with 3-MeV proton beams resulting in high resolution carbon maps, however, the count rate for nitrogen and oxygen was too low. The results demonstrate that on thin samples, 36-MeV C4+ will produce good quality PIXE spectra in less time; therefore, carbon ions may be advantageous depending on which element is being studied. However, these advantages may be outweighed by the inherent disadvantages including increased ion beam damage, the necessity of very high ion energies resulting in higher neutron fields.

PIXE/RBS as a tool to study cementitious materials: Application to the dynamic leaching of concrete

The suitability of the application of Ion Beam Analysis (IBA) techniques such as Particle Induced X-ray Emission spectrometry (PIXE) and Rutherford Backscattering Spectrometry (RBS) to elemental depth profiling in concrete is analysed, studying hardened samples of concrete prior to and after a dynamic leaching test. A calibration of the data has been done by comparing the results obtained by IBA techniques with those obtained by Chemical and Thermogravimetric Analysis (TG/DTA). From PIXE and RBS data relevant information about the migration of minor elements, within the concrete matrix after leaching is obtained.

Application of ion beam analysis to the selective sublimation processing of thin films for gas sensing

Ion beam analysis was successfully applied to a novel technique, named selective sublimation process (SSP), for deposition of nanostructured gas-sensing films through reactive sputtering. The method consists of the co-deposition of a mixed oxide, one of which has a relatively low sublimation temperature. Annealing at suitable temperature causes the sublimation of the most volatile compound, leaving a layer with adjustable composition. The appropriate choice of thermal treatments and the consequent tailoring of the composition play a crucial role in the determination of the microstructural properties.We developed a model based on diffusion equations that provides a useful guide to control the deposition and processing parameters and we applied the model on the systems TiO2–WO3 and TiO2–MoO3. Rutherford backscattering (RBS) was demonstrated to be effective for the characterization of the diffusion and sublimation processes during SSP. Experimental results fully agree with theoretical prediction, and allowed the calculation of all the parameters involved in SSP.

Application of ion beam analysis for the control of the improvement of the oxidation resistance of TiAl at 900 °C in air by fluorine ion implantation and HF-treatment

The oxidation resistance of TiAl at elevated temperatures >750°C can be improved by the addition of small amounts of fluorine. The fluorine is applied in two ways: ion implantation and wetting with diluted HF. Using non-destructive Ion Beam Analysis the fluorine depth concentration profiles in the near surface region are determined before and after oxidation. The fluorine maximum is found to be at the metal/oxide interface, which supports the theoretical explanation of the fluorine microalloying effect. The time dependent behaviour of the fluorine content is characterized by a fast decrease of the fluorine concentration during the first hours of oxidation followed by a moderate decrease. The results offer the possibility for a technical application of the fluorine microalloying effect to improve the oxidation resistance of TiAl-alloys at temperatures >750°C.

Application of ion beam analysis to the characterization of protective coatings prepared by plasma detonation techniques on steel samples

Ion beam analysis was used in order to characterize Al2O3 layers deposited on stainless steel by plasma detonation techniques and Al2O3/Cr/TiN composite protective coatings. The aluminum depth distribution was determined using the 991keV resonance of the 27Al(p,γ)28Si reaction, whereas the 14N(d,α)12C reaction was utilized for the nitrogen profiling. The determination of the titanium depth distribution was performed by Rutherford backscattering spectrometry (RBS). The ratio of Al:O and Ti:N in the investigated Al2O3 and TiN layers was found to be close to the stoichiometric one. The effect of an additional high current electron beam (HCEB) treatment on the composition of the coatings was also investigated. Titanium and nitrogen diffusion from the surface to the interior was observed in the case of the coatings treated by HCEB.

Electronic stopping of He, B, N, and Al in SiC

Silicon carbide (SiC) is a wide-band-gap semiconductor that has attracted extensive investigations for a wide range of device applications. Accurate values of stopping powers in SiC, especially for B, N, and Al ions as dopants and for He ions used in ion-beam analysis applications, are highly desirable. In the present study, the electronic energy loss of these ions in a self-supported SiC film is directly measured in transmission geometry using a time-of-flight detection system over a continuous range of energies. The measured electronic stopping powers are parameterized, for easy implementation in other applications, and compared with the predictions of the stopping and range of ions in matter code.

Characterization of calcium phosphate bioceramic films using ion beam analysis techniques

The analytical techniques using ion beams are powerful tools for surface analysis of solid materials. Constituent elements are important in determining the biocompatibility and corrosion resistance of a biomaterial implant. The focus of this article is on the application of ion beam analysis towards quantifying the composition of calcium phosphate based biomaterials. Thin films of calcium phosphate bioceramics were prepared on Si and Ti substrates using ion beam sputter deposition (IBSD) and ion beam assisted sputter deposition (IBASD) methods. Precise amounts of calcium, phosphorus, oxygen and hydrogen in these thin films are determined by combining four ion beam analysis techniques. The simultaneous application of proton induced X-ray emission (PIXE) and Rutherford backscattering spectrometry (RBS) were utilized to quantify composition and amounts of elements heavier than helium. Elastic recoil detection analysis (ERDA) was used to determine hydrogen content while resonance-enhanced RBS (RE-RBS) was utilized to measure oxygen concentration. The amount of assisting ion beam current density during deposition affected the concentration ratios of Ca, O and H to P. Combination of different ion beam analysis methods is useful in characterizing the elemental composition and distribution of composite biomaterials.

Ion beam analysis at cryogenic temperatures for polymer light emitting diodes

The application of ion beam analysis on polymer light emitting diodes became possible by the development of a set-up which allows measurements at cryogenic temperatures (10–30 K). The set-up is equipped with a sample holder which combines compatibility with a load-lock, necessary for introduction of samples under controlled conditions, and a good thermal contact. A number of examples are reviewed in which interface stability and oxidation effects in poly-LEDs are studied with Rutherford backscattering spectrometry and elastic recoil detection.

Modelling the sorption of mercury (II) on (hydr)oxides: Application of ion beam analysis to sorption processes

The sorption of a heavy metal — mercury (II) — on two naturally occurring oxides: anatase (TiO 2) and vernadite (δ-MnO 2) is studied here. Mercury sorption (II) data were modelled with the help of the commonly used surface complexation model. The results obtained were then compared with spectra obtained by ion beam analysis in order to gather further information on sorption mechanisms.

Bayesian techniques and the principle of maximum entropy in ion-beam analysis applications

The Bayesian Formalism (BF) and the principle of Maximum Entropy (MaxEnt) are applied to techniques relevant to Ion-Beam Analysis (IBA). The BF is an efficient and theoretically sound method of information recovery, and when applied together with an entropic prior it has special applications in solving ill-posed inverse problems, e.g. the deconvolution of the detector response function from PIXE or RBS spectra. Results include the recovery of depth profiles in PIXE using a two-detector set-up. The deconvolution of RBS spectra using the BF is also compared to more conventional deconvolution techniques, namely Fourier Transforms and the non-linear Jansson method.

The application of ion beam analysis to calcium phosphate‐based biomaterials

The application of ion beam analysis to calcium phosphate‐based biomaterials