Ion Beam Analysis Techniques Research Articles

Influence of the hydrogen content on the optical properties of TiOx thin films

In this work, dark Ti(OxH)y films were obtained by DC magnetron reactive sputtering under different oxygen partial pressures (PO2) starting from a high base pressure chamber atmosphere (10−5 mbar) with the purpose of investigating the visible light absorption dependence of the hydrogen content and stoichiometry. The TiOx film compositions, thicknesses, and elemental depth profiles were measured by ion beam analysis (IBA) techniques in a self-consistent approach. The optical properties were investigated by visible and near-infrared spectrophotometry, and the crystallography was examined by small-angle X-ray diffraction. The films deposited at a low PO2 were dark, and as the partial oxygen pressure increases, they became transparent. The IBA showed that the hydrogen content exponentially decreased as the PO2 increased. The optical constants for the films, n and k, are dependent on oxygen and hydrogen ratio as well as the optical band gap that can be modulated from 0.40 to 3.25 eV, and thus a significant improved PEC activity. These modulations may be useful for optical or electronic devices as a variable semiconductor or dielectric layer.

Ion beam analysis of fusion plasma-facing materials and components: facilities and research challenges

Following the IAEA Technical Meeting on ‘Advanced Methodologies for the Analysis of Materials in Energy Applications Using Ion Beam Accelerators’, this paper reviews the current status of ion beam analysis (IBA) techniques and some aspects of ion-induced radiation damage in materials for the field of materials relevant to fusion. Available facilities, apparatus development, future research options and challenges are presented and discussed. The analysis of beryllium and radioactivity-containing samples from future experiments in JET or ITER represents not only an analytical but also a technical challenge. A comprehensive list of the facilities, their current status, and analytical capabilities comes alongside detailed descriptions of the labs. A discussion of future issues of sample handling and the current status of facilities at JET complete the technical section.To prepare the international IBA community for these challenges, the IAEA technical meeting concludes the necessity for determining new nuclear reaction cross-sections and improving the inter-laboratory comparability by defining international standards and testing these via a round-robin test.

Analysis of Ancient Glass Using Ion Beams and Related Techniques

Ion Beam Analysis (IBA) techniques are established as an indispensable tool for material analysis. They are very powerful when applied to the examination of uniform layers. In recent years they have been also used for the quality control of implanted layers, which improve the mechanical or chemical properties of common materials. The use of IBA techniques for the study of corrosion is impeded by the non-uniformity of such layers, which renders the analysis difficult. In the Material Analysis Laboratory of the Institute of Nuclear Physics, a combination of experimental techniques and analytical algorithms has been developed, which allows the non-destructive examination of corrosion layers on cultural artifacts. Ancient glass fragments from Kenchreai, Greece, were analyzed with ion beam techniques, in order to examine the applicability of the latter to the characterization of the surface. The relative distribution of heavy components was determined by X-Ray Fluorescence (XRF). Nuclear reactions were used to determine the depth distribution of H, O, C and Si. The Hydrogen distribution rises sharply from the surface, reaching a maximum of 9xl022 at/cm3 at 0.5 μπι and then decays smoothly to a depth of approximately 2 μπα. Examination of the same samples with aparticles, indicates a depletion of Silicon in the same surface region, while the Oxygen distribution is uniform. A detailed analysis, using the 28Si(p, p) reaction, which resonates at 2.095 MeV, confirms the depletion and other non-uniformities in the Silicon distribution.

Change in Li depth profiles of Au/LCO/mixed LATP-LAGP/Pt battery under discharging studied by ion beam analysis techniques with 9 MeV O4+ ions

Li depth profiles in Au/LCO/mixed LATP-LAGP/Pt battery (mixed LATP-LAGP (LATP/LAGP) = Li1+X+YAlYTi2−YGeXP3−XO12, LCO = LiCoO2) under discharging by biasing Pt to Au at earth potential, have been measured from both Au and Pt surfaces by means of reflection elastic recoil detection (ERD) and Rutherford backscattering spectrometry (RBS) techniques with 9 MeV O4+ ions. Ge and Ti compositions of a mixed LATP-LAGP electrolyte and thickness of LCO were determined from RBS spectrum for the as-prepared specimen, where Y and X in LATP were estimated to be 0.84 and 1.27, respectively. On charging at 2.4 V for 25 min, Li composition in LCO measured from the Au surface by ERD was reduced down to ~0.3 and hereafter on discharging at 0.5 V for 25 min the composition was not enriched, but contrary was further reduced to 0.2. However, by successive discharging at 1.0, 1.5 and 2.2 V for 50 min the composition was enriched. On the other hand, it was found from the Pt surface that Li charged in the electrolyte near Pt by biasing at 2.4 V for 20 min was reduced by discharging at 1.0 V for 20 min. By further discharging for 20 min Li was not reduced, but contrary was enriched. Both anomalous transports of Li under discharging are discussed in terms of diffusion of Li atoms in the counter direction to the biasing which is caused by the transport fraction of Li ions in the electrolyte less than unity.

Li depth profiles of metal/Li-electrolyte/metal capacitors under biasing studied by means of MeV ion beam analysis techniques

Li Depth profiles at the interfaces of capacitors of Cu/LiPON/Cu and Al/LiPON/Al prepared on buffer Ti layer /SiO2glass and Au/LATP/Au (LiPON = Li3.3PO3.8N0.2, LATP = Li3.1Al0.84Ti1.16Ge1.27P1.73O12) under biasing bottom metal against top metal at earth potential have been in-situ measured by means of elastic recoil detection analysis (ERD) and Rutherford backscattering spectrometry (RBS) techniques. Li has been found to be enriched near the interface with electrode biased negatively, while it is depleted near that biased positively. The Li depth profile in electrolyte has been theoretically calculated, taking into account the transport faction of Li ions, based on hopping diffusion model of Li ions under potential gradient. It is shown that the Li depth profile calculated as a solution of diffusion equation at steady state agrees qualitatively well with the experimental ones and the transport fraction of Li ions in electrolyte is less than unity.

W and Tl M-shell X-ray production cross sections induced by carbon ions of energy between 1.56 MeV and 5 MeV

Although PIXE is usually performed with protons, PIXE with heavier ions can be useful in some specific cases. A number of Ion Beam Analysis (IBA) techniques, like ERDA (Elastic Recoil Detection Analysis), NRA (Nuclear Reaction Analysis), AMS (Accelerator Mass Spectrometry), or MeV-SIMS (MeV Secondary Ion Mass Spectrometry), require the use of heavier ions. In such cases the simultaneous use of PIXE could be beneficial. One of the prerequisites for such use of PIXE is good knowledge of X-ray production with heavier ions. In order to update the data base of heavy ion X-ray production cross sections, we have recently started with the systematic study of M-Shell X-ray production induced by carbon ions on heavy elements between W and Bi. Following previous works on Au and Pb (Haidra et al., 2018) and Pt and Bi (Haidra et al., 2019). In this work, we have measured particularly Mαβ, Mγ and total M-shell X-ray production cross section in tungsten and thallium induced by carbon ions of energy range 1.56 MeV to 5 MeV on respective thin targets. The obtained new experimental data are compared to the theoretical predictions given in the framework of the models Plane Wave Born Approximation (PWBA) (Brandt and Lapicki, 1981), ECPSSR (Brandt and Lapicki, 1981) and the Semi-Classical Approximation with united atom (SCA-UA) and separated atom (SCA-SA) correction (Bang and Hansteen, 1957) [5].

Long-term variations of the elemental concentration of table cream

Nowadays, most of the food available for human consumption goes through some sort of processing before reaching the table of consumers. Usually, modern societies consume packed food preserved in cardboard boxes and cans. In the context of food science and technology, analytical techniques capable of characterizing the elemental composition of foodstuff and their respective containers are a powerful tool to monitor modifications over time. In particular, ion beam analytical techniques like Particle-Induced X-ray Emission (PIXE) have already been employed in the investigation of canned food, providing valuable information about the interaction of food and its container.In this work, the PIXE technique was employed in order to study the elemental composition of canned table cream focusing on variations occurred over several years of production as well as on the possible diffusion of Fe from the cans to the table cream as a function of the storage time of the product.The qualitative analysis showed the presence of 10 characteristic elements in the table cream, with prevalence of potassium and calcium. Bromine and rubidium were found in some samples as well. For long storage times, it was observed a rising trend for the concentration of iron in the product. Moreover, the analysis indicated a sudden rise in the levels of sodium and chlorine, which could indicate an adulteration of the product.

Determination of Deposition Order of Toners, Inkjet Inks, and Blue Ballpoint Pen Combining MeV-Secondary Ion Mass Spectrometry and Particle Induced X-ray Emission.

Determination of the deposition order of different writing tools is very important for the forensic investigation of questioned documents. Here we present a novel application of two ion beam analysis (IBA) techniques: secondary ion mass spectrometry using MeV ions (MeV-SIMS) and particle induced X-ray emission (PIXE) to determine the deposition order of intersecting lines made of ballpoint pen ink, inkjet printer ink, and laser printer toners. MeV-SIMS is an emerging mass spectrometry technique where incident heavy MeV ions are used to desorb secondary molecular ions from the uppermost layers of an organic sample. In contrast, PIXE provides information about sample elemental composition through characteristic X-ray spectra coming from greater depth. In the case of PIXE, the information depth depends on incident ion energy, sample matrix and self-absorption of X-rays on the way out from the sample to the X-ray detector. The measurements were carried out using a heavy ion microprobe at the Ruđer Bošković Institute. Principal component analysis (PCA) was employed for image processing of the data. We will demonstrate that MeV-SIMS alone was successful to determine the deposition order of all intersections not involving inkjet printer ink. The fact that PIXE yields information from deeper layers was crucial to resolve cases where inkjet printer ink was included due to its adherence and penetration properties. This is the first time the different information depths of PIXE and MeV-SIMS have been exploited for a practical application. The use of both techniques, MeV-SIMS and PIXE, allowed the correct determination of deposition order for four out of six pairs of samples.

Investigation of chloramphenicol release from PVA/CMC/HEA hydrogel using ion beam analysis, UV and FTIR techniques

PVA/CMC/HEA based cross-linked hydrogels were synthesized. These were utilized as matrix chloramphenicol drug releasing systems. Combination of different analytical techniques was applied to understand drug releasing process. Ion beam analysis (IBA) measurements, namely micro-PIXE analysis, were applied to gain information regarding spatial distribution of chloramphenicol within the system. Independent complement measurements utilizing UV and pore volume measurements were also employed to additionally characterize and verify the experimental findings obtained by IBA techniques. FTIR was utilized to both characterize and justify the releasing behavior of the crosslinked systems. Comprehensive literature comparison between different analytical methods has been reviewed.

RBS, PIXE, Ion-Microbeam and SR-FTIR Analyses of Pottery Fragments from Azerbaijan

The present work is aimed at the investigation of the ceramic bulk and pigmented glazed surfaces of ancient potteries dating back to XIX century A.D. and coming from the charming archeological site located in the Medieval Agsu town (Azerbaijan), a geographic area of special interest due to the ancient commercial routes between China, Asia Minor, and Europe. For the purpose of the study, complementary investigation tools have been exploited: non-destructive or micro-destructive investigation at elemental level by ion beam analysis (IBA) techniques, by using Rutherford Backscattering Spectrometry (RBS), Proton-Induced X-ray Emission (PIXE) spectroscopy and ion-microbeam analysis, and chemical characterization at microscopic level, by means of synchrotron radiation (SR) Fourier transform infrared (FTIR) microspectroscopy. The acquired information reveals useful for the identification of the provenance, the reconstruction of the firing technology, and finally, the identification of the pigment was used as a colorant of the glaze.

Elastic backscattering as a method for the measurement of the integral lithium content in thin films on fusion-relevant substrates

Different ion beam analysis techniques for the study of thin lithium-containing layers on top of fusion relevant materials are discussed and compared to each other. Elastic backscattering analysis (EBS) with protons is determined to be one of the most promising techniques and allows measurements of Li layers with thicknesses from ∼100 nm up to ∼600 μm, as shown by SIMNRA simulations. The best sensitivity for thin films (∼100 nm) can be achieved using 4 MeV protons with 170° scattering detection angle for layers on Mo and W substrates, and 2 MeV for C substrates. Experimentally EBS measurements were successfully tested for Li films with thicknesses from ∼50 nm up to ∼400 nm after air exposure. The Li films become strongly inhomogeneous and require averaging over multiple measurements in nearby areas. This necessitates averaging over multiple nearby measurement points, and limits the overall precision of the measurement.

Superintense Laser-driven Ion Beam Analysis

Ion beam analysis techniques are among the most powerful tools for advanced materials characterization. Despite their growing relevance in a widening number of fields, most ion beam analysis facilities still rely on the oldest accelerator technologies, with severe limitations in terms of portability and flexibility. In this work we thoroughly address the potential of superintense laser-driven proton sources for this application. We develop a complete analytical and numerical framework suitable to describe laser-driven ion beam analysis, exemplifying the approach for Proton Induced X-ray/Gamma-ray emission, a technique of widespread interest. This allows us to propose a realistic design for a compact, versatile ion beam analysis facility based on this novel concept. These results can pave the way for ground-breaking developments in the field of hadron-based advanced materials characterization.

Rf design studies on the 750 MHz radio frequency quadrupole linac for proton-induced x-ray emission analysis

The proton-induced x-ray emission (PIXE) is the most commonly used ion beam analysis technique. It allows for nondestructive quantitative elemental characterization and is used in a variety of fields, particularly for the diagnosis of cultural heritage artwork. To provide mobile access to PIXE, a compact transportable radio frequency quadrupole (RFQ) linac has been designed and is being built at CERN. The PIXE RFQ has a length of only one meter and accelerates a proton beam to an energy of 2 MeV. This paper covers various rf design studies for the RFQ operating at 750 MHz. We show simulation results regarding cavity, equipment, and coupler geometry. Thermomechanical and beam dynamics studies are presented as well. The paper concludes with a conceptual study on dipole mode detuning by means of length adjustment.

Laser-PIXE using laser-accelerated proton beams

Laser-driven proton acceleration is a field of growing interest, in particular for its numerous applications, including in the field of materials science. A benefit of these laser-based particle sources is their potential for a relative compactness in addition to some characteristics at the source that differ from those of conventional, radio-frequency based proton sources. These features include, e.g., a higher brilliance, a shorter duration, and a larger energy spread. Recently, the use of laser-accelerated protons has been proposed in the field of Cultural Heritage, as alternative source for the Particle Induced X-ray Emission diagnostic (“laser-PIXE”), a particular ion beam analysis (IBA) technique that allows to precisely analyse the chemical composition of the material bulk. In this paper we study the feasibility of the laser-PIXE using laser-accelerated proton beams. We focus on materials specifically of interest for the Cultural Heritage domain. Using Geant4 simulations, we show that the laser-PIXE allows analysing a larger volume than conventional PIXE, profiting from the large energy spread of laser-accelerated protons. Furthermore, for specific materials, the large energy spread allows investigating multilayer materials, providing an advantage compared to conventional PIXE technologies.

Investigation of tungsten-coated divertor tiles at the JET tokamak with the ITER‐Like Wall

Materials migration in fusion plasma devices and fuel retention in plasma-facing components are issues of great importance for the safe operation of fusion devices. The underlying mechanisms require a good understanding in order to make predictions regarding the lifetime of wall components and to assess the amount of fuel retained in the machine mainly in co-deposited layers. To reduce fuel inventory and to investigate plasma-wall interactions a large-scale experiment at the JET (Joint European Torus) tokamak is realized: operation with the ITER-Like Wall (JET-ILW) which comprises beryllium and tungsten. The current work reports on the post-mortem analysis of W/CFC tiles retrieved after the first deuterium-deuterium campaign at JET-ILW. Specimens from different areas of the divertor have been analyzed by means of several techniques including nuclear reaction analysis and Rutherford backscattering employing a deuterium beam. In addition, X-ray fluorescence spectroscopy and scanning electron microscopy with energy dispersive X-ray analysis are used to assess the sample surface morphology and analyze the stoichiometry of the surface of the samples in order to compare with the results from the ion beam analytical techniques.

Development of a simulation code for material analysis using the PIGE technique

Particle Induced Gamma ray Emission (PIGE) is a well known and widely used Ion Beam Analysis (IBA) technique for non-destructive material analysis, usually in conjunction with Proton Induced X-ray Emission (PIXE). The main drawback in the applicability of PIGE regarding the quantification of light elements in various heavy element substrates is the need for many reference targets with similar matrices to the one under study, because of the importance of the ion energy loss in the calculations. In order to overcome this problem, an appropriate simulation code that uses as inputs the experimental spectrum and the relevant differential cross sections, with the output being the quantification of the concentration depth profiles of the isotopes of interest is needed. A code like this is currently being developed in C++ and it is compatible with Windows, Linux and Mac.

Structure and morphology of copper oxide composite materials synthesized by the arc discharge method

Copper oxide is a semiconducting compound with a narrow band gap and is used for photoconductive and photothermal applications. Most of the synthesis methods for the preparation of copper oxide composite materials either are unsuitable for mass fabrication or inevitably introduce unwanted impurities. In this work, we report on the synthesis of copper oxide composite materials by the arc discharge method with a pure copper rod as the anode and graphite as the cathode. Ion beam analysis techniques, particle-induced X-ray emission and Rutherford backscattering spectrometry were used to probe the impurities in the copper oxide composites. Ion beam analysis results revealed copper and oxygen as constituent elements with no impurities. X-ray diffraction results discovered the presence of CuO, Cu2O and Cu phases in the composite materials. The morphology of the as-synthesized copper oxide was studied by scanning electron microscopy. Results clearly demonstrated that spherical particles were obtained with an average diameter of 14 [Formula: see text]m (range 2–85 [Formula: see text]m), 35 [Formula: see text]m (range 20–100 [Formula: see text]m) and 50 [Formula: see text]m (range 30–120 [Formula: see text]m) for the arc current of 60 A, 80 A and 95 A, respectively. It was found that the morphology can be controlled by the arc discharge parameters, e.g. a lower arc discharge current contributed to a smaller particle size. This is because the electric arc current influences the nucleation and the growth of the spherical structures. Due to its simplicity of synthesis, the proposed arc discharge is a promising technique for the fabrication of copper oxide composite materials for optical and electrical applications.

Fatigue Behaviour of Additive Manufactured Ti-TiB

ABSTRACTFatigue behaviour of titanium reinforced with TiB particles fabricated by ‘plasma transferred arc solid freeform fabrication’ (PTA-SFFF) technique was investigated. Rotation bending fatigue tests were conducted following the MPIF 56 standard using the staircase method approach. Experimental data is used to calculate the fatigue strength and construct S-N curves, where the results were compared to a powder metallurgy FC0205 as a benchmark material. The titanium samples were found to exhibit superior fatigue behaviour in comparison to the reference FC0205 material, performing well above 1/3 of its ultimate tensile strength with a 90% survival fatigue strength of 244 +/- 98.3 MPa versus 141 +/- 17.4 MPa. Fatigue failure mechanisms of samples were identified by examination of the fracture surfaces through scanning electron microscopy (SEM) as well as using transmission-electron microscopy (TEM) and focused ion beam (FIB) analysis techniques. Fatigue crack propagation was either arrested or deflected when propagation occurred within the vicinity of the TiB intermetallics. Fracture surfaces of the titanium matrix displayed evidence of striations while the TiB intermetallic experience cleavage fracture.

Full elemental depth-profiling with nanoscale resolution: The potential of Elastic Recoil Detection (ERD) in membrane science

Extensive characterization is needed to understand how the physicochemical properties of polymeric membranes are related to their transport properties and to allow optimization of membrane design. Currently, most techniques characterize the (near)-surface region of the membrane, even though its bulk obviously also plays a significant role in the final membrane performance. To achieve depth-profiles of the elemental composition of both integrally skinned asymmetric (ISA) and thin-film composite (TFC) membranes, elastic recoil detection (ERD), an ion beam analysis technique, is now introduced to the field as a potentially highly valuable tool to complement for instance XPS, EDX or RBS. The determination of the complete elemental composition, importantly also including hydrogen, as function of the membrane thickness allows to gain knowledge about its depth-heterogeneity at an impressive combination of ca. 15 nm resolution with ppm-range sensitivity. This very low detection limit additionally allows the analytical quantification of e.g. remnants from synthesis conditions. The potential as well as the pitfalls of ERD as a novel, valuable technique for membrane characterization are critically discussed and illustrated by the determination of the thickness of polyamide-based top-layers of TFC membranes.

Towards a portable X-ray luminescence instrument for applications in the Cultural Heritage field⋆

Analytical techniques based on luminescence properties of materials have proved to be useful in the study of artistic and archaeological materials. For example, iono-luminescence (IL), in conjunction with ion beam analysis (IBA) techniques, and cathodoluminescence (CL), coupled with optical microscopy or scanning electron microscopy (SEM), are important for identifying mineral phases and provenance studies. X-ray luminescence (XRL) has been used on Cultural Heritage less than other luminescence techniques; we therefore investigated its potential in this field. The first developed setup, necessarily to be used in the laboratory, was tested on a provenance study of the lapis lazuli “Savoy Collection”, kept by the Regional Museum of Natural Sciences in Turin. Very interesting results were obtained: while some samples were labelled as Chilean origin (or simply no attribution), XRL spectra clearly excluded that particular provenance for any specimen of the collection. Although this approach has given valuable information, the potentiality of the technique has not yet been fully exploited due to lack of portability, a great limitation for characterising ancient artefacts. We therefore upgraded the sensitivity of our detection setup, in order to respond also to lower signal levels obtainable with portable X-ray sources. The first results are encouraging and comparable with those obtained with non-portable setups.