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Dear Visitor,
The workshop on “Multi-probe imaging for materials” will take place at the European Synchrotron research facility, Grenoble, from September 22nd to 24th. It is sponsored by the ReMade@ARI EU project (www.remade-project.eu) with the participation of DragonFly.
In this workshop, we aim to bring together experts from various imaging modalities, such as X-rays, electrons and neutrons, and to present their applicability in material science (Please see the full aims and scope).
The workshop consists of two plenary days and an optional tutorial day. It includes a series of presentations, a poster session, a visit to the imaging beamlines of ESRF, hands-on tutorials provided by DragonFly and SPAM, and a gala dinner in the vibrant city of Grenoble.
This workshop presents an opportunity for the participants to discuss with the beamline and instrument scientists about their projects and potentially use Remade or ESRF proposal channel to carry out their research.
Should our workshop spark your curiosity, then wait no longer. The organization committee members are very excited to welcome you to this workshop and have a fruitful scientific discussion.
This sponsored event aims to keep costs reasonable at 100€ for regular participants and 50€ for PhD students (lunch & gala dinner included). Travel support for young scientists linked to ReMade proposals is available, see below*.
* Ten bursaries are available for PhD students and young scientists associated with an existing ReMade application (preproposal or full proposal) coming from a ReMade partner country (EU, UK, CH). The bursaries will contribute towards your travel and accommodation expenses (max 600 Euros as 300 for travel and 50 Euros per night; reimbursed after participation in the event). The aim of these bursaries is to help ReMade users gain knowledge of the programme or about specific techniques and to give them an opportunity to interact with the scientists who would help them during experiments. Contact the workshop organisers to ask for this support and tell them why attending the workshop could be beneficial for your research. Bursaries will be allocated by the organisers at their discretion.
Organisers
Jaianth Vijayakumar (ESRF),
Zhenggang Zhang (ESRF),
Miguel Sequeira (HZDR),
Yan Lu (FZ Jülich GmbH),
Masoud Dialameh (IMEC),
Gary Admans (ESRF)
Anne-Françoise Maydew (ESRF)
Mylène Le Caer (ESRF)
With participation of:
Abstract attached
Content in attached word abstract
X-ray Fluorescence Ghost Imaging (XRF-GI) was recently demonstrated for x-ray lab sources. It has the potential to reduce acquisition time and deposited dose by choosing their trade-off with spatial resolution, while alleviating the focusing constraints of the probing beam. In this talk, we present the realization of synchrotron-based XRF-GI: We present both an adapted experimental setup and its corresponding required computational technique to process the data.
In particular, we present a new self-supervised deep-learning-based GI reconstruction method (called Noise2Ghost), which provides unparalleled reconstruction performance for noisy acquisitions among unsupervised methods. Self-supervision removes the need for clean reference data while offering strong noise reduction. This provides the necessary tools for addressing signal-to-noise ratio concerns for GI acquisitions in emerging and cutting-edge low-light GI scenarios.
In conclusion, the highlights of our work are:
• Extension of the above-mentioned potential advantages of GI to synchrotron XRF imaging.
• A new strategy to improve resilience against drifts at all scales, and the study of previously inaccessible samples, such as liquids.
• A potential new avenue for the development of micro- and nano-scale x-ray emission imaging with dose-sensitive samples.
Notable applications that could benefit from our work include in-vivo and in-operando case studies for biological samples and batteries.
Three-dimensional elemental mapping at nanometer-scale resolution by atom probe tomography (APT)
M. Dialameh1, J. Scheerder1, R. Morris1, and C. Fleischmann1,2
1 imec, Kapeldreef 75, 3001 Leuven, Belgium
2 KU Leuven, Department of Physics and Astronomy, Quantum Solid-State Physics, 3001 Leuven, Belgium
masoud.dialameh@imec.be
Advances in atom probe tomography (APT) have expanded its capabilities beyond conventional applications in metal alloys, enabling diverse types of analyses across a broader range of material systems, including complex semiconductors, advanced catalysts, battery and sustainable energy materials, each highly relevant to the circular economy. The developments are driven by the unique capability of APT to combine three-dimensional nanometer-scale spatial resolution with isotopically precise elemental identification of both heavy and light elements, including hydrogen [1]. These strengths enable diverse types of materials analysis, including voxel-based 3D compositional mapping with a sensitivity approaching parts-per-million level depending on the voxel volume [1]; detection and characterization of solute clusters, precipitates, and segregated regions as small as ~1 nm [2]; nearest-neighbour distribution analysis; and proximity histograms for quantitative interface characterization.
APT operates on the principle of controlled field evaporation from a needle-shaped specimen. During analysis, surface atoms are sequentially ionized, accelerated in a strong electric field, and detected by a position-sensitive detector coupled with time-of-flight mass spectrometry. Subsequent data analysis and three-dimensional reconstruction of the detected ions allow the original atomic arrangement within the specimen to be resolved, under ideal conditions. This provides atomic-scale insights from local, nanometer-sized regions of a material, in contrast to most X-ray based techniques that yield ensemble-averaged measurements. In practice, however, accurate APT analysis of complex material systems faces several challenges, including reliable specimen preparation, preferential ion evaporation in heterogeneous systems, and data reconstruction artifacts.
This presentation will provide a brief introduction to the fundamentals of APT, covering field evaporation, specimen preparation, and three-dimensional data reconstruction. A selected case studies of APT analysis on semiconductors and metal alloys will be presented, with the emphasis on potentials and the challenges of applying APT to such material systems.
References
[1] Gault, Baptiste, et al. "Atom probe tomography." Nature Reviews Methods Primers 1.1 (2021): 51.
[2] De Geuser, Frédéric, and Baptiste Gault. "Metrology of small particles and solute clusters by atom probe tomography." Acta Materialia 188 (2020): 406-415.
The new generation of synchrotron sources offers the ultimate state-of-the-art instrumentation in terms of resolution, brilliance and coherence. Coupled with a nano-probe, it allows new mechanisms and processes to be studied in materials sciences and engineering. Beamline ID16B at the ESRF - The European Synchrotron - proposes a multi-modal approach al-lowing the combination of several nano-scale techniques such as X-ray fluorescence (XRF), X-ray absorption spectroscopy (XANES), X-ray diffraction (XRD), X-ray Excited Optical Luminescence (XEOL), X-ray Beam Induced Current (XBIC) and 3D phase contrast nano-imaging. The presentation will detail the use of synchrotron X-ray nano-tomography to understand the mechanical response of an additively manufactured Al alloy with heterogenous microstructures.
Indeed, the microstructures of aluminum alloys designed for laser beam powder bed fusion (LB-PBF) can be heterogeneous across all scales. A bimodal grain structure is often observed with fine-grained regions (FG) consisting of submicron grains near the melt pool boundaries, and coarser columnar grains (CG) in the melt pool interiors. In the FG and CG regions, the morphology and size of intermetallic particles differ as does the composition of the solid solution due to changes in local solidification conditions at the melt pool scale. This specific grain arrangement leads to a 3D architecture at the mesoscale. The mechanical response of such microstructures was found to be influenced by the microstructure heterogeneity using digital image correlation based on SEM images collected during in situ tensile tests. The response of such heterogeneous microstructures is affected by the relative mechanical behaviour of the FG and CG regions.
However, the complexity of the microstructure topology requires a 3D approach to further improve our understanding of the mechanical response of such Al alloys. Thanks to 3D images collected using synchrotron X-ray nano-tomography (voxel size of 25nm3) at the beamline ID16B after different strain increments, we determined the 3D strain maps, at the scale of few melt pools, in a high strength aluminum alloy designed for LB-PBF. The high resolution of the 3D images allowed capturing the fine intermetallic network decorating the microstructure. This enabled to perform high resolution digital volume correlation (DVC) since these intermetallics act as a natural speckle and allow subsets as small as 2 µm3 to be used. The evolution of the 3D strain fields as a function of the macroscopic stress is considered and the heterogenous distribution of strain is explored.
We present an integrated approach for high-precision sorting and characterisation of electronic components from E-waste by combining machine vision, X-ray absorption spectroscopy imaging and machine-learning classification. This study demonstrates the effectiveness of optical sorting based on machine vision coupled with classification algorithms such as convolutional neural networks (CNN). This combination allows similar electronic components to be efficiently grouped together, making them easier to recycle. In addition to optical sorting, X-ray absorption spectroscopy is being introduced to overcome the limitations of optical sorting by providing crucial information on the elemental composition of electronic components. The integration of these sorting methods into a single process, supported by the construction of a prototype, demonstrates the relevance of this approach, demonstrating up to 96.9% accuracy. The overall process offers the opportunity not only to group similar electronic components efficiently, but also to significantly enrich the final streams with targeted elements, enabling the recovery of previously lost elements due to their low concentration in electronic waste with elemental enrichments by up to 10,000 for targeted elements. This study opens the door to large-scale industrial application of the process, making it economically viable to recycle many elements of interest.
Our dependence to electronic tools has made the supply of critical raw metals (CRMs) crucial. Waste printed circuit boards (PCBs) is a promising source of such CRMs, but most of the latter are not recoverable with current industrial recycling practices. One major issue to be solved: the overall composition, and therefore the value, of this urban mine comprising of PCBs. Indeed, this is necessary for stakeholders to build accurate and viable business models to mitigate criticality issues and enable their recycling. To solve this, one need to build a database of the chemical composition of the millions of electronic components (ECs) to be found in such e-wastes. However, full-element analysis of ECs lacks standardization in literature and is often proprietary piece of information from electronic manufacturers.
Hence, our team propose to demonstrate the feasibility of high throughput X-ray fluorescence imaging of waste ECs using synchrotron radiation to populate a reference database of ECs (@BM23, ESRF). This would enable online estimation of the e-waste flux composition, and educated sorted strategies toward sorting bin that are simpler, less variable and more concentrated in targeted CRMs.
Our team also investigate hard x-ray hyperspectral scans as signatures to access a reference components entries in the database. Such scan is acquired online using a transmission setup with an x-ray tube and a pixelated photon counting detectors, and provide a more unique, composition-related signature than an RGB image.
ESRF main building first floor
Globally, the annual demand for primary aluminium (Al) is estimated at ∼70 million tons and the uses of secondary Al or recycled Al consume only ∼7% of the energy compared to the primary Al.
Hence, it is vital to maximise the reuses and recycling rate of secondary Al to reduce the greenhouse gas emissions in Al industry.
In almost all commercial Al alloys, Fe is the most common detrimental element, which is often accumulated in the sorting and remelting processes and form different type of brittle Fe-rich intermetallic phases, damaging greatly castability and mechanical properties of the alloys.
it is critical to develop efficient and effective methodologies to restrict the detrimental Fe phases or to modify/change the damaging phase morphology into beneficial ones in order to improve the mechanical properties.
Here, I present the recent operando research work of using the fast synchrotron X-ray diffraction and tomography techniques at the ESRF plus machine-learning assisted phase segmentation methods to study the 3D nucleation dynamics of the Fe phases in a typical multiple-component recycled Al alloy; and how co-growth of the multiple Fe phases lead to the formation of the complex and convoluted 3D Chinese-script phases.
In addition, the beneficial effects of applying ultrasound to control the primary Al dendrites and to alter the Fe phase growth dynamics as well as the final 3D morphology were also discussed and elucidated in this work.
Electrostatic potential, including both that contributed by electron-beam-induced specimen charging and intrinsic material-related mean inner potential (MIP), is crucial because it is influence the reaction between charged particles, chemical reactivity, and dielectric properties. Off-axis electron holography is a powerful TEM technique that can be used to map local variations in electron optical phase shift, which are in turn sensitive to electrostatic potentials and magnetic fields. In the absence of magnetic contributions to the phase shift, the recorded phase is proportional to the projected electrostatic potential within and outside the specimen. Insulating nanoparticles with simple geometries are ideal objects for the study of specimen charging in the TEM.
Polystyrene latex beads were examined temperature-dependent behavior of the MIP and electron-beam-induced charge from room temperature down to 5.3 K in a FEI Titan G2 TEM at 300 kV. The diameter of latex spheres is in the range of 230 nm to 600 nm. By using a model-independent approach for the quantification of the spatially-dependent projected charge density from a recorded phase image [1,2], the amount of positive charge on the sphere at each temperature was determined. Isolating the electrostatic potential contributed by the electron-beam-induced charge, the MIP was obtained at high precision, revealing a significant increase of 16.8% as temperature decreases from RT to 5 K.
In addition, this talk will present the quantification of electron-beam-induced charge on MgO nanocubes reflecting the amount of oxygen vacancies on the surface, which is essential for catalytical reaction [3].
Bacteria and other microorganisms form biofilms upon and within materials, affecting their physical and chemical properties, such as pore-scale clogging, mineral precipitation, or gas production. Upon the surface, biofilms can be studied by electron and optical microscopy. However, within opaque materials, other techniques such as micro-computed tomography (µCT) are necessary. Unfortunately, biofilms consist of water and other light materials, making them nearly indistinguishable from water. Contrast-Enhancing Staining Agents (CESAs) can improve visualization, but existing CESAs mainly stain the water phase, can precipitate, are toxic, or are time-consuming. In our research, five CESAs: Mono-WD POM, Hf-WD 1:2 POM, isotonic Lugol, Hexabrix® and CA4+ were evaluated for their ability to enhance the contrast of biofilms with conventional lab-based µCT. Two CESAs, Hf-WD 1:2 POM and isotonic Lugol, effectively increased the attenuation and contrast of the biofilm. It enabled the visualization of biofilms that could otherwise not be (fully) visualized. It included cyanobacterial biofilms colonizing sandstone [1] and biofilms of heterotrophic bacteria colonizing the pores of sand filters [2] (Fig. 1). Isotonic Lugol produced stronger attenuation but may induce shrinkage, whereas Hf-WD 1:2 POM could potentially induce swelling. Furthermore, spectral CT at TESCAN XRE was applied to further confirm the uptake of iodine (for biofilms stained with isotonic Lugol) and tungsten and hafnium (for biofilms stained with Hf-WD 1:2 POM) and to enhance further discrimination between the phases. While iodine signals correlated clearly with biofilm presence, tungsten and hafnium detection were less consistent. Future research should focus on the CESA-biofilm interaction and apply these CESAs within the industrial and research fields. Initial experiments have already been conducted in the scope of the BugControl project at Utrecht University and within the EXCITE Transnational Access at Ghent University.
The formability of Al2050 alloy is critical for manufacturing large and thick components while maintaining its outstanding performance [1]. Previous studies showed that pores and cracks occur during the hot deformation of this alloy and the pore growth follows three different paths (exponential, decelerated, mixed) [2]. To link the damage development during high-temperature loading with the alloy microstructure evolution, an in-situ tensile loading at 480 ºC was performed on this alloy using synchrotron diffraction and tomography, i.e. diffraction contrast tomography (DCT) to provide 3D grain maps at ~1.1 µm resolution and phase contrast tomography (PCT) to characterize pores and intermetallic phases with 0.55 µm voxel size and scanning 3DXRD (s3DXRD) to obtain 2D grain and elastic strain maps at 0.5 µm resolution. The pore density and volume fraction were quantified as a function of macroscopic strain up to 20% and three pore formation mechanisms were identified: growth from pre-existing pores, fracture of the intermetallic particles, and nucleation of new pores. The characteristics of the pore evolution are then linked with the grain structure (grain boundaries, orientations and strains) characterized by DCT and s3DXRD. Additionally, the grain maps show newly recrystallized grains, suggesting the presence of dynamic recrystallization. To exclude the possible explanation by annealing recrystallization, an in-situ annealing experiment at 480 ºC without external loading was performed and the results confirmed no recrystallized grains. This study demonstrates that correlating synchrotron grain mapping techniques with tomography offers comprehensive insight in linking the damage development with the microstructure evolution under high-temperature deformation.
References
[1] M.J. Couper, A.E. Neeson and J.R. Griffiths, Fatigue Fract. Engng Mater. Struct. 13, 213-227 (1990).
[2] A.A. Harrup Gutierrez, PhD Thesis (2024).
Copper-Indium-Gallium-di-Selenide or CIGS panels are one of the promising alternatives in the market for thin-film solar technologies. CIGS panels are lightweight, durable and use less semiconductor materials as compared to Si-based PV modules [1, 2]. According to EU CRM materials report 2023, indium gallium and copper which are raw materials for CIGS panels are rated as critical or strategic materials subject to their high supply risk and moderate economic importance [3]. The development of robust recycling methodologies for copper indium gallium selenide (CIGS) photovoltaic panels and associated production waste presents a viable pathway towards securing the supply of critical raw materials (CRMs). While a range of recycling processes have been explored, many current approaches demonstrate limitations. Specifically, challenges remain in achieving both efficient material separation and high material purity within a single process. Furthermore, certain methodologies necessitate operation under highly toxic conditions, resulting in the generation of secondary waste streams which require further management. Within this research electrochemical leaching for separation and recovery of materials from CIGS solar panels is studied. The scope of study is to determine efficiency of semicomductor coating separation from glass in H3C-SO2-OH (Methanesulphonic Acid). Using ICP-OES/MS and XPS techniques the dissolution and de-coating efficiencies are calculated. The investigation includes the observing effective separation of the glass and coating material at different acid concentrations in novel drum electrode[4].Furthremore, studies have been conducted to recover Cu from mixed CRMs solution in high purity. Purity upto 98% for Cu was achieved. Further optimisation of parametes is needed to improve purity and yeild. Within the study, sustainability analysis of the processes from ecological, safety and social aspects are briefly discussed.
References
[1] A. M. Gustafsson, "Recycling of CIGS solar cell waste materials," Chalmers University of Technology, Gothenburg Sweden, 2014.
[2] J. Cartwright, "Better, more versatile silicon-free solar cell technologies," Horizon: The EU research and Innovation Magazine, 16 10 2013. [Online]. Available: https://ec.europa.eu/research-and-innovation/en/horizon-magazine/better-more-versatile-silicon-free-solar-cell-technologies. [Accessed 08 10 2022].
[3] European Commission, "Study on the EU's list of Critical Raw Materials 2023," European Commission, Brussels, 2023.
[4] H. Khadse; Choi, B.; D’Souza, A.; Wickleder, M.; Beck G. Rotary drum electrode for electrochemical recycling of composite materials, FEMS Euromat, 2023
The material characterization by neutron imaging reached a new level after developing innovative techniques using different contrast mechanisms than the common beam attenuation. In this way properties of materials and complex systems can be resolved by position sensitive mapping of diffraction, small-angle scattering and refraction signals. In addition, the improved spatial and time resolution of the detector systems allows for micro tomography studies and 3D dynamic investigations.
Applications related to 2D and 3D visualization of material phase heterogeneities, texture, fluid dynamics, magnetic structures and phase transitions in applied materials will be presented [1].
A new-generation of synthetic bone scaffold is tailored using a bricks-and-mortar approach from bioactive glass nanoparticles BGNps (SiO2-CaO-P2O5 doped with metal ions, the bricks), and customized polymers (PLA, poly (lactic acid), the mortar). Used as synthetic implants for substitutive and regenerative therapies targeting mandibular osteoradionecrosis (ORM), they must promote bone formation and cell adhesion, while exhibiting high porosity, adequate mechanical strength, and pro-angiogenic coupled with antibacterial properties. Freeze-casting solutions of BGNps and PLA derivatives can result in hybrid nanocomposite scaffolds1, with a multi-scale porosity, offering improved mechanical properties and proper auto-catalytic degradation.
To shed light on the mechanisms behind the formation of the hierarchical structure of these scaffolds, the synthesis of BGNps derived from Stöber silica was studied using in-situ SAXS at synchrotron facilities (ID02@ESRF2 and SWING@SOLEIL). The SAXS data revealed the preorganization of the particles in solution prior to freeze-casting.
Subsequently, thanks to a custom-built sample chamber, fast X-ray phase-contrast tomography operando experiments were performed using synchrotron beams (ID19@ESRF). They allowed to follow the controlled growth via a freeze-casting process of centimeter-cubed scaffolds made from nanoparticles (bricks) and polymers (mortar), at high resolution. We pictured the fabrication process from the initial suspension of nanoparticles to the finalized porous material, obtained via lyophilization that was also studied operando with X-ray tomography.
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