Integrating Non-Destructive Ion Beam Analysis Methods and AMS Radiocarbon Dating for the Study of Ancient Bronze Statues

Analytical methods based on particle accelerators are widely used in cultural heritage diagnostics and archaeological sciences from the absolute dating of organic materials by means of radiocarbon accelerator mass spectrometry (AMS) to the analysis of the elemental composition of a wide range of materials (metals, obsidians, pottery) via ion beam analysis (IBA) techniques. At CEDAD (Centre for Dating and Diagnostics), the accelerator facility of the University of Salento, AMS 14C dating and PIXE (particle-induced X-ray emission)-PIGE (particle-induced gamma-ray emission) compositional analysis in external beam mode are combined to study certain archaeological materials. We present a review of the combined application of these analytical methods in the study of casting cores of the Riace bronzes, 2 classical Greek statues of extraordinary importance for the history of art.

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A New High-Throughput Focused MeV Ion-Beam Analysis Setup

Instruments ◽

10.3390/instruments5010010 ◽

2021 ◽

Vol 5 (1) ◽

pp. 10

Author(s):

Sören Möller ◽

Daniel Höschen ◽

Sina Kurth ◽

Gerwin Esser ◽

Albert Hiller ◽

...

Keyword(s):

Gamma Ray ◽

Rutherford Backscattering Spectrometry ◽

Ion Beam ◽

Complete Analysis ◽

Nuclear Reaction Analysis ◽

Beam Optics ◽

Single Measurement ◽

Ion Beam Analysis ◽

Beam Analysis ◽

Technical Solutions

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.

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Absolute Local Quantification of Li as Function of State-of-Charge in All-Solid-State Li Batteries via 2D MeV Ion-Beam Analysis

Batteries ◽

10.3390/batteries7020041 ◽

2021 ◽

Vol 7 (2) ◽

pp. 41

Author(s):

Sören Möller ◽

Takahiro Satoh ◽

Yasuyuki Ishii ◽

Britta Teßmer ◽

Rayan Guerdelli ◽

...

Keyword(s):

Solid State ◽

Lithium Batteries ◽

Gamma Ray ◽

Ion Beam ◽

State Of Charge ◽

Ex Situ ◽

Lithium Content ◽

Emission Analysis ◽

Ion Beam Analysis ◽

Beam Analysis

Direct observation of the lithiation and de-lithiation in lithium batteries on the component and microstructural scale is still difficult. This work presents recent advances in MeV ion-beam analysis, enabling quantitative contact-free analysis of the spatially-resolved lithium content and state-of-charge (SoC) in all-solid-state lithium batteries via 3 MeV proton-based characteristic x-ray and gamma-ray emission analysis. The analysis is demonstrated on cross-sections of ceramic and polymer all-solid-state cells with LLZO and MEEP/LIBOB solid electrolytes. Different SoC are measured ex-situ and one polymer-based operando cell is charged at 333 K during analysis. The data unambiguously show the migration of lithium upon charging. Quantitative lithium concentrations are obtained by taking the physical and material aspects of the mixed cathodes into account. This quantitative lithium determination as a function of SoC gives insight into irreversible degradation phenomena of all-solid-state batteries during the first cycles and locations of immobile lithium. The determined SoC matches the electrochemical characterization within uncertainties. The presented analysis method thus opens up a completely new access to the state-of-charge of battery cells not depending on electrochemical measurements. Automated beam scanning and data-analysis algorithms enable a 2D quantitative Li and SoC mapping on the µm-scale, not accessible with other methods.

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RECENT DEVELOPMENTS IN THE AIR PARTICULATE RESEARCH CAPABILITY AT THE NEW ZEALAND ION BEAM ANALYSIS FACILITY

International Journal of PIXE ◽

10.1142/s012908351240013x ◽

2012 ◽

Vol 22 (01n02) ◽

pp. 121-130 ◽

Cited By ~ 2

Author(s):

B. BARRY ◽

W. J. TROMPETTER ◽

P. K. DAVY ◽

A. MARKWITZ

Keyword(s):

New Zealand ◽

Elemental Analysis ◽

Analytical Methods ◽

Ion Beam ◽

Sampling System ◽

Great Flexibility ◽

Ion Beam Analysis ◽

Air Particulate ◽

Beam Analysis ◽

Recent Developments

The New Zealand capability in Ion Beam Analysis of air particulate samples has been upgraded in recent years. The main equipment change has been the introduction of the ability to analyse samples taken using the Streaker (PIXE International Corporation) sampling system. This is an automated sampler which allows for great flexibility in monitoring programmes by collecting particulates for up to about 70 sampling periods which can range in collection times from seconds to many hours. The IBA analysis for hydrogen on standard filters and for PIXE multi-elemental analysis of the Streaker filters has also been studied with a view to optimising analytical methods.

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