Search Results (10)

Sputtering of silicon in a He magnetron discharge (MS) has been reported as a bottom-up procedure to obtain He-charged silicon films (i.e., He nanobubbles encapsulated in a silicon matrix). The incorporation of heavier noble gases is demonstrated in this work with a synergistic effect, producing increased Ne and Ar incorporations when using He–Ne and He–Ar gas mixtures in the MS process. Microstructural and chemical characterizations are reported using ion beam analysis (IBA) and scanning and transmission electron microscopies (SEM and TEM). In addition to gas incorporation, He promotes the formation of larger nanobubbles. In the case of Ne, high-resolution X-ray photoelectron and absorption spectroscopies (XPS and XAS) are reported, with remarkable dependence of the Ne 1s photoemission and the Ne K-edge absorption on the nanobubble’s size and composition. The gas (He, Ne and Ar)-charged thin films are proposed as “solid” targets for the characterization of spectroscopic properties of noble gases in a confined state without the need for cryogenics or high-pressure anvils devices. Also, their use as targets for nuclear reaction studies is foreseen. Full article

Surface laser treatment (SLT) using nanosecond IR lasers has been shown to improve the tribological behaviour of titanium. Here, we studied the fretting wear of SLT-functionalized pure titanium in a mixture of reactive gases O${}_2$ (20 vol.%) + N${}_2$ (80 vol.%). The contact geometry was a ball on a plane and the ball was made of bearing steel. The very small amplitude of relative displacement between reciprocating parts in fretting wear makes the evacuation of wear particles difficult. Moreover, the oxidation mechanism of the debris depends on the accessibility of the surrounding atmosphere to the tribological contact. This work focused in the analysis of debris generation and oxidation mechanisms, and sought to differentiate the role of oxygen forming part of the ambient O${}_2$ + N${}_2$ gas mixture from oxygen present in the surface layer of the SL-treated titanium. Before the fretting test, the surface of the commercially pure titanium plates was treated with a laser under a mixture of O${}_2$ + N${}_2$ gases with oxygen enriched in the ${}^{18}$O isotope. Then, the fretting tests were performed in regular air containing natural oxygen. Micro-Raman spectroscopy and ion beam analysis (IBA) techniques were used to analyse the TiO${}_2$ surface layers and fretting scars. Iron oxide particles were identified by Raman spectroscopy and IBA as the third body in the tribological contact. The spatial distribution of ${}^{18}$O, Ti, ${}^{16}$O and Fe in the fretting scars was studied by IBA. The analysis showed that the areas containing high concentrations of Fe displayed also high concentrations of ${}^{16}$O, but smaller concentrations of ${}^{18}$O and Ti. Therefore, it was concluded that tribological contact allows the oxidation of iron debris by its reaction with ambient air. Full article

Ion beam analysis (IBA) methods refer to a set of analytical techniques based on the interactions of energetic ions, produced by a particle accelerator, with matter. The result of such interactions is the emission of characteristic radiation, X and gamma rays, and charged particles, which, upon detection, provide valuable information on the absolute concentration and depth distribution of the elements in the bombarded material. Moreover, IBA techniques can be performed while maintaining the object to be investigated at atmospheric pressure, without placing it in vacuum, in an analysis chamber, with the impinging ion beam extracted from the in-vacuum beamline of the accelerator, avoiding the need of invasive sampling and greatly easing the object positioning, thus allowing precious and big or large artefacts to be studied. This feature has opened the way for applications of IBA techniques for compositional analysis in cultural heritage studies, providing detailed and complete information about elemental compositions and depth distributions of analysed materials that are otherwise difficult or impossible for other analytical techniques. In this paper, the basic principles of the main IBA techniques applied to cultural heritage, namely, particle induced X-ray emission (PIXE), particle induced Gamma-ray emission (PIGE), and Rutherford or elastic backscattering spectrometry (RBS/EBS), will be recalled, and specific and practical details on how these techniques can be used for analysing cultural heritage objects with external beam set-ups will be provided. Full article

The Ethiopian magic scrolls are traditional parchment artifacts used by the Christians of Ethiopia as protection against disease and demonic possessions. On the occasion of their restoration in the Accademia delle Belle Arti di Bologna (Italy); a preliminary characterization before the treatments has been performed on four Ethiopian scrolls belonging to the Archivio storico della provincia di Cristo Re dei Frati Minori dell’Emilia Romagna of Bologna (Italy). In order to plan an effective preservative restoration procedure and; at the same time; to investigate the manufacturing techniques; the text and the decorations on the magic scrolls were studied and characterized. A combined approach by imaging and compositional techniques was used: Infrared Reflectography (IRR) for the preliminary characterization of the graphic supports and the identification of the points to sample the chemical measurements; and the spectroscopic analyses to clarify the hypothesized investigations and confirm the chemical composition of the inks. In particular; Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) spectroscopy has provided information relating to the molecular composition of inks and pigments; while a characterization of the constituent elements is obtained with the Ion Beam Analysis (IBA). The ink composition proved to be consistent with data generally documented in the literature and contributing to the expansion of knowledge on Ethiopian magic scrolls and their production. Full article

Analytical techniques play a fundamental role in heritage science. Among them, Particle Induced X-ray Emission (PIXE) and X-ray Fluorescence (XRF) techniques are widely used in many laboratories for elemental composition analysis. Although they are well-established, a strong effort is put on their upgrade, making them suitable for more and more applications. Over the years, at the INFN-LABEC (the laboratory of nuclear techniques for the environment and cultural heritage of the Italian National Institute of Nuclear Physics), the INFN-CHNet group, the network devoted to cultural heritage, has carried out many technological improvements to the PIXE and XRF set-ups for the analysis of works of art and archaeological finds. Among the many, we recall here the scanning external microbeam facility at the TANDEM accelerator and the MA-XRF scanner. The two instruments have shown complementary features: the former permits quantitative analysis of elements heavier than sodium, which is not possible with the latter in most of the case studies. On the contrary, the scanner has the undeniable advantage of portability, allowing it to work in situ. In this framework of technological developments in heritage science, INFN, CERN, and OPD are jointly carrying on the MACHINA (Movable Accelerator for Cultural Heritage In-situ Non-destructive Analysis) project for on-site Ion Beam Analysis (IBA) studies on cultural heritage. Full article

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. Full article

Forgeries exist in many fields. Money, goods, and works of art have been imitated for centuries to deceive and make a profit. In the field of Cultural Heritage, nuclear techniques can be used to study art forgeries. Ion beam analysis (IBA), as well as ¹⁴C accelerator mass spectrometry (AMS), are now established techniques, and the purpose of this paper is to report on their capacity to provide information on ancient, as well as modern, forgeries. Two case studies are presented: the production of silver counterfeit coins in the 16th century and the detection of recent forgeries of 20th century paintings. For the counterfeit coins, two silvering processes were identified by IBA: mercury silvering (also called amalgam silvering or fire silvering) and pure silver plating. The discovery of 14 mercury silvered coins is an important finding since there are very few known examples from before the 17th century. In the detection of recent forgeries, among the five paintings examined, ¹⁴C dating showed that three of them are definitely fakes, one is most likely a fake, and one remains undetermined. These results were obtained by using the bomb peak calibration curve to date canvas and paint samples. Full article

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, SiO_x-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 SiO_x. 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. Full article

The analysis of material composition by ion-beam analysis (IBA) is becoming a standard method, similar to electron microscopy. A pool of IBA methods exists, from which the combination of particle-induced-X-ray emission (PIXE), particle induced gamma-ray analysis (PIGE), nuclear-reaction-analysis (NRA), and Rutherford-backscattering-spectrometry (RBS) provides the most complete analysis over the whole periodic table in a single measurement. Yet, for a highly resolved and accurate IBA analysis, a sophisticated technical setup is required integrating the detectors, beam optics, and sample arrangement. A new end-station developed and installed in Forschungszentrum Jülich provides these capabilities in combination with high sample throughput and result accuracy. Mechanical tolerances limit the device accuracy to 3% for RBS. Continuous pumping enables 5 × 10⁻⁸ mbar base pressure with vibration amplitudes < 0.1 µm. The beam optics achieves a demagnification of 24–34, suitable for µ-beam analysis. An in-vacuum manipulator enables scanning 50 × 50 mm² sample areas with 10 nm accuracy. The setup features the above-mentioned IBA detectors, enabling a broad range of analysis applications such as the operando analysis of batteries or the post-mortem analysis of plasma-exposed samples with up to 3000 discrete points per day. Custom apertures and energy resolutions down to 11 keV enable separation of Fe and Cr in RBS. This work presents the technical solutions together with the quantification of these challenges and their success in the form of a technical reference. Full article

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. Full article