A knob bow fibula (Bügelknopffibel) of the Leutkirch type, which typologically belongs to the second half of the 4th and early 5th century CE, was excavated in 2018 in the Roman city of Augusta Raurica, present-day Kaiseraugst (AG, Switzerland). This was analyzed for the first time for its elemental composition by using the non-destructive technique of Muon Induced X-ray Emission (MIXE) in the continuous muon beam facility at the Paul Scherrer Institute (PSI). In the present work, the detection limit is 0.4 wt% with $$\sim$$ ∼ 1.5 hours of measurement time. The fibula was measured at six different positions, at a depth of 0.3–0.4 mm inside the material. The experimental results show that the fibula is made of bronze, containing the main elements copper (Cu), zinc (Zn), tin (Sn) and lead (Pb). The compositional similarities/differences between different parts of the fibula reveal that it was manufactured as two “workpieces”. One workpiece consists of the knob (13.0±0.6 wt% Pb), bow (11.9±0.4 wt% Pb) and foot (12.5 ± 0.9 wt% Pb). These show a higher Pb content, suggesting a cast bronze. The spiral (3.2 ± 0.2 wt% Pb), which is part of the other workpiece, has a comparatively lower Pb content, suggesting a forged bronze.

The usage of muonic x-rays to study elemental properties like nuclear radii ranges back to the seventies. This triggered the pioneering work at the Paul Scherrer Institute (PSI), during the eighties on the Muon-induced x-ray emission (MIXE) technique for a non-destructive assessment of elemental compositions. In recent years, this method has seen a rebirth, improvement, and adoption at most muon facilities around the world. Hereby, the PSI offers unique capabilities with its high-rate continuous muon beam at the Swiss Muon Source (SμS). We report here the decision-making, construction, and commissioning of a dedicated MIXE spectrometer at PSI, the GermanIum Array for Non-destructive Testing (GIANT) setup. Multiple campaigns highlighted the outstanding capabilities of MIXE at PSI, e.g., resolving down to 1 at. % elemental concentrations with as little as 1 h data taking, measuring isotopic ratios for elements from iron to lead, and characterizing gamma rays induced by muon nuclear capture. On-target beam spots were characterized with a dedicated charged particle tracker to be symmetric to 5% with an average σ = 22.80(25) and 14.41(8) mm for 25 and 45 MeV/c, respectively. Advanced analysis of the high-purity germanium signals further allows us to improve energy and timing resolutions to ∼1 keV and 20 ns at 1 MeV, respectively. Within the GIANT setup, an average detector has a photopeak efficiency of $\overline{{ϵ}_E}=0.11$ % and an energy resolution of $\overline{{\sigma }_E}=0.8\text{keV}$ at E = 1000 keV. The overall performance of the GIANT setup at SμS allowed us to start a rich user program with archaeological samples, Li-ion battery research, and collaboration with the industry. Future improvements will include a simulation-based analysis and a higher degree of automation, e.g., automatic scans of a series of muon momenta and automatic sample changing.

The toolbox for material characterization has never been richer than today. Great progress with all kinds of particles and interaction methods provide access to nearly all properties of an object under study. However, a tomographic analysis of the subsurface region remains still a challenge today. In this regard, the Muon Induced X-ray Emission (MIXE) technique has seen rebirth fueled by the availability of high intensity muon beams. We report here a study conducted at the Paul Scherrer Institute (PSI). It demonstrates that the absence of any beam time-structure leads to low pile-up events and a high signal-to-noise ratio (SNR) with less than one hour acquisition time per sample or data point. This performance creates the perspective to open this technique to a wider audience for the routine investigation of non-destructive and depth-sensitive elemental compositions, for example in rare and precious samples. Using a hetero-structured sample of known elements and thicknesses, we successfully detected the characteristic muonic X-rays, emitted during the capture of a negative muon by an atom, and the gamma-rays resulting from the nuclear capture of the muon, characterizing the capabilities of MIXE at PSI. This sample emphasizes the quality of a continuous beam, and the exceptional SNR at high rates. Such sensitivity will enable totally new statistically intense aspects in the field of MIXE, e.g., elemental 3D-tomography and chemical analysis. Therefore, we are currently advancing our proof-of-concept experiments with the goal of creating a full fledged permanently operated user station to make MIXE available to the wider scientific community as well as industry.

Battery research often encounters the challenge of determining chemical information, such as composition and elemental oxidation state, of a layer buried within a cell stack in a non-destructive manner. Spectroscopic techniques based on X-ray emission or absorption are well-suited and commonly employed to reveal this information. However, the attenuation of X-rays as they travel through matter creates a challenge when trying to analyze layers buried at depths exceeding hundred micrometers from the sample's surface. In the context of battery research, the limited escape depth of X-rays often imposes to design experiment-specific cells with thinner inner layers, despite the risk that these tailored cells may not exactly replicate the cycling behavior of larger commercial cells. Muon-induced X-ray emission (MIXE) is a non-destructive spectroscopic technique that involves implanting negative muons into a sample and detecting the highly energetic muonic X-rays generated when these muons are captured by the sample's atoms. By virtue of the high energy of muonic X-rays, the depth of analysis of MIXE greatly exceeds other X-ray based techniques. In this article, we introduce the technique and lay the groundwork for employing MIXE in future in-situ/operando analyses of batteries. We demonstrate that MIXE can detect nearly all elements, including low atomic number ones such as Li. Additionally, we establish the quantitative nature of MIXE through the precise determination of LiNi_xMn_yCo_1-x-yO₂ (NMC) electrode stoichiometries. Finally, we demonstrate that MIXE enables the acquisition of depth-resolved chemical information from 100-1,000 μm thick cells, in good agreement with simulation results.

The specific depth‐profiling capabilities of the muonic x‐ray emission spectroscopy (μ‐XES) technique have proved to be effective for examination of the elemental distribution within ancient coins. This ‘layered’ analysis can also be applied to the examination of ancient faience, the production of which can result in distinct layers (glaze, interaction, and body). Initial results also indicated the presence of nitrogen and carbon, something with potential implications for production techniques of these objects. Moreover, by using this method, the samples do not become radioactive. This paper presents a pilot study of this method used on three faience samples, two from the Nubian (ancient Sudanese) site of Meroe (c.350 bce –350 ce ) and one from the ancient Egyptian site of Beni Hasan (c.2055–1650 bce ).