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What does GD-OES reveal about the aging and manufacturing processes of lithium-ion batteries?
(2024)
Glow-Discharge Optical Emission Spectroscopy (GD-OES), a powerful analytical technique, sheds light on the two critical aspects of lithium-ion batteries (LIBs): manufacturing and aging 1, 2. We optimized cell production in manufacturing by adjusting parameters, including cathode doping, electrolyte concentration, and pressing force. GD-OES provided in-depth elemental composition and homogeneity analysis, which is crucial for identifying optimal manufacturing conditions. These findings were validated by electrochemical impedance spectroscopy, confirming the quality of the manufactured batteries.
Shifting the focus to aging, we use GD-OES for fluorine depth profiling, a key element in understanding polymer and electrolyte degradation. However, fluorine presents analytical challenges. We addressed this by substituting argon with a neon:argon mixture, which significantly enhanced fluorine detection sensitivity. This advancement not only improves accuracy but also holds the potential to guide sustainable and cost-efficient manufacturing strategies.
Through its versatility, GD-OES has proven to be a powerful tool for not only optimizing LIB manufacturing processes but also gaining deeper insights into their aging mechanisms. This research extends beyond academic interest, offering tangible benefits for the industry by translating into improved battery quality, extended lifespan, and overall performance.
An artificial digestion of silver nitrate is reported. It is shown that AgSCN nanoparticles emerge from ionic silver in saliva and remain present during the entire digestion process. The particles were characterized by infrared spectroscopy and small- and wide-angle X-ray scattering (SAXS/WAXS) regarding their composition and size distribution.
The earliest known recipes for iron gall inks include four basic ingredients: oak galls – pathological growths of oak leaves; metal salts – usually referred to as vitriol; a binder such as gum Arabic; and water. The final product differs in the elemental composition due to the multitude of recipes as well as differences within the composition of the ink’s ingredients. Nowadays, based on the qualitative and semi-quantitative evaluation of X-ray fluorescence data, it is possible to distinguish inks on the basis of the so-called fingerprint model. The first goal of our study was to determine to what extent the type of XRF spectrometer affects the quality of the ink evaluation. We tested two types of spectrometers, semi-stationary machines equipped with polycapillary focusing optics and a handheld spectrometer with a diaphragm collimator and a relatively big interaction spot.
The second goal was to address the issue of whether the ink composition might be affected by storage in a metal container. The presentation will discuss the role of the spectrometer type in the evaluation of a thin layer material such as ink.
We have also learned that the iron-gall ink composition might depend on the type of vessel in which ink was being stored.
Zinc is an essential trace element and is ingested daily by humans, partly in dissolved form. The first contact is with saliva, in which many ions are dissolved whose solubility product with zinc can be low. This could result in compounds forming, possibly in nanoparticular form, which could have different effects on the organism than pure zinc ions.
In this study, we report on the saliva stage of the artificial digestion of zinc chloride as a model substance for zinc ions. To facilitate in situ measurements, the sample is continuously passed through a small-angle x-ray scattering (SAXS) system. This custom-made machine is capable of measuring over a wide q-range and thereby able to resolve structures from around 250 nm down to the crystal structure. It is thus an excellent tool for investigating both the particle size distribution and the atomic structure of the sample.
By curve fitting, we found that shortly after addition of zinc chloride to saliva, small particles with a mean radius of 1.9 ± 0.1 nm and a distribution width of 0.6 ± 0.1 nm formed. These particles are aggregated to compact mass fractals with a fractal aggregate size of 14.7 ± 0.1 nm and a fractal dimension of 2.96 ± 0.02. Approximately 7200 single particles form each mass fractal, whose radius of gyration was found to be 36 ± 1 nm. The growth of these structures continues over the course of several weeks. To determine the compound that was formed, infrared spectroscopy was used in addition to the SAXS measurements, and zinc phosphate was identified as the product.
This talk introduces the expanded view that comes from wide-range X-ray scattering investigations.
Compared to X-ray diffraction studies alone, the additional angular range of this technique provides information on the larger structural dimensions present in your samples. This allows for the extraction of information on the size and size distribution of nanostructural components, such as nanoparticles, nanovoids, and any other structure exhibiting an electron density contrast.
The talk introduces the technique, the MOUSE instrument used for these investigations, and provides several real-world examples of its uses. The audience is invited to choose which examples captures their interest from a range of options, in the latter segment of the talk.
The paper addresses “WHITE LIGHT INTERFERENCE MICROSCOPY, ELLIPSOMETRY, AND INSTRUMENTED INDENTATION TESTING AS REFERENCE PROCEDURES“ and is subdivided in the following sections: 1. Measurement vs. testing vs. reference procedures, 2. White light interference microscopy (WLIM) for determination of step height h, 3. Spectroscopic ellipsometry (SE) for determination of layer thickness d and 4. Instrumented indentation testing (IIT) for determination of indentation hardness HIT. The following points are discussed in more detail: methodology of measurement and testing, uncertainty budgets for direct (WLIM), model-based (SE) and formula-based (IIT) reference procedures by means of specific examples. It is shown that standardization efforts are connected to reference procedures.
Aging Mechanisms of Lithium Batteries: How can we make batteries more durable and more sustainable in the future?
Lithium batteries are particularly susceptible to ageing processes. During each charging and discharging process in an electric battery, lithium ions are deposited in the electrodes of the cell like in the pores of a sponge. Over time, however, fractures and cracks occur in the filigree structures. The result: more and more lithium ions no longer fit into the hollow spaces of the „sponge“, instead they accumulate in heaps around the electrodes and hinder the movement of other ions. The performance of the battery decreases.
We present our new project, in which we are developing a fast and cost-effective method with which companies that produce lithium batteries can already assess the ageing behaviour of their batteries in the laboratory.
While studying the socio-geographic history of inks, division 4.5 (Analysis of cultural artefacts and assets) of the BAM (Bundesanstalt für Materialforschung und -prüfung) in Berlin together with the Centre for the Study of Manuscript Cultures in Hamburg has developed a protocol for ink analysis. It consists of a primary screening to determine the type of the ink, and a subsequent in-depth analysis using several spectroscopic techniques.
Using this protocol, scientists can assist scholars in addressing a rather broad range of historical questions that cannot be answered unequivocally through scholarly research alone. Among these are investigations on collaboration between scribes and scriptoria, on the usage and annotation of manuscripts and on their path through time and space in general. This research can thus help to reconstruct the circumstances of the production of written heritage as well as their history and transmission.
To facilitate the dialogue between the scholars and the scientists a simple optical tool was developed to allow the scholars to perform preliminary ink analysis required for formulation of the question that in turn can be answered by scientific in-depth investigations. In this paper, ink types and their identification method is accompanied by examples of the recent work conducted on parchment manuscripts in the Austrian National Library.
Modern wind turbine rotor blades consist of sandwich shell segments made from glass fiber reinforced polymers. During manufacturing, defects can arise which could lead to failure of the whole component under dynamic mechanical and thermal loads. Hence during operation defects can arise which, if detected, can be repaired locally and in-situ by applying repair patches instead of taking the whole rotor blade down and repair it remotely. This method is much more time and cost effective, since the shut-down time of the energy converter is limited to a minimum. These repair patches can, however, also lead to new defects if not applied optimally. Therefore, it is necessary to control the quality of the repair patches to ensure the best possible restoration of structural integrity of the component. As a rotor blade is an object with a large aspect ratio, X-ray laminography is predestined to provide 3D information of the objective volume. To enhance the amount of information gained from laminographic reconstruction, we use in this study a photon counting and energy discriminating X-ray detector and apply a material decomposition algorithm to the data. By inherently separating the incident spectra within the detection process into two distinct energy bins, the basis material decomposition can provide material resolved images. Choosing glass and epoxy resin as basis materials and numerically solving the inverse dual-energy equation system, the reconstructed laminographic datasets contain highly valuable information about the distribution of the basis materials within the structure. Furthermore, cross- artifacts arising from the limited angle of the projection data can be reduced by this method which allows to investigate structures that were hidden underneath the artefacts.
Modern wind turbine rotor blades consist of sandwich shell segments made from glass fiber reinforced polymers. During manufacturing, defects can arise which could lead to failure of the whole component under dynamic mechanical and thermal loads. Hence during operation defects can arise which, if detected, can be repaired locally and in-situ by applying repair patches instead of taking the whole rotor blade down and repair it remotely. This method is much more time and cost effective, since the shut-down time of the energy converter is limited to a minimum. These repair patches can, however, also lead to new defects if not applied optimally. Therefore, it is necessary to control the quality of the repair patches to ensure the best possible restoration of structural integrity of the component. As a rotor blade is an object with a large aspect ratio, X-ray laminography is predestined to provide 3D information of the objective volume. To enhance the amount of information gained from laminographic reconstruction, we use in this study a photon counting and energy discriminating X-ray detector and apply a material decomposition algorithm to the data. By inherently separating the incident spectra within the detection process into two distinct energy bins, the basis material decomposition can provide material resolved images. Choosing glass and epoxy resin as basis materials and numerically solving the inverse dual-energy equation system, the reconstructed laminographic datasets contain highly valuable information about the distribution of the basis materials within the structure. Furthermore, cross- artifacts arising from the limited angle of the projection data can be reduced by this method which allows to investigate structures that were hidden underneath the artefacts.
Shape memory alloy structures for actuator and vibration damper applications may be manufactured using wire arc additive manufacturing (W AAM), which is one of the additive manufacturing technologies. Multilayer deposition causes heat accumulation during W AAM, which rises the preheat temperature of the previously created layer. This leads to process instabilities, which result in deviations from the desired dimensions and mechanical properties changes. During W AAM deposition of the wall structure, a systematic research is carried out by adjusting the interlayer delay from 10 to 30 s. When the delay period is increased from 10 to 30 s, the breadth decreases by 45% and the height increases by 33%. Grain refinement occurs when the interlayer delay duration is increased, resulting in better hardness, phase transformation temperature, compressive strength, and shape recovery behavior. This study shows how the interlayer delay affects the behavior of W AAM-built nickel-titanium alloy (NiTi) structures in a variety of applications.
In this study, nanoscopic particles of magnesium Fluoride (MgF2) and calcium fluoride (CaF2) also known as nano metal fluorides (NMFs), were evaluated for their potential to improve wood durability. Even though these fluorides are sparingly soluble, their synthesis in the form of nano-sized particles turns them into promising candidates for wood preservation. Their distinct property of low-water solubility is proposed to maintain long-lasting protection of treated wood by reducing the leaching of fluoride. Analytical methods were used to characterize the synthesized NMFs and their distribution in treated wood specimens. Transmission electron microscopy images showed that these fluoride particles are smaller than 10 nm. In nano metal fluoride (NMF) treated specimens, aggregates of these particles are uniformly distributed in the wood matrix as confirmed with scanning electron microscopy images and their corresponding energy-dispersive X-ray spectroscopy maps. The fluoride aggregates form a protective layer around the tracheid walls and block the bordered pits, thus reducing the possible flow path for water absorption into wood. This is reflected in the reduced swelling and increased hydrophobicity of wood treated with NMFs. The biocidal efficacy of NMFs was tested against brown-rot fungi (Coniophora puteanaand Rhodonia placenta), white-rot fungus (Trametes versicolor), and termites (Coptotermes formosanus). The fungal and termite tests were performed in accordance with the EN 113 (1996) and EN 117 (2012) standards, respectively. Prior to fungal tests, the NMF treated wood specimens were leached according to the EN 84 (1997)standard. Compared to untreated specimens, the NMF treated wood specimens have a higher resistance to decay caused by brown-rot fungi, white-rot fungus, and termites. Although all NMF treatments in wood reduce the mass loss caused by fungal decay, only the combined treatment of MgF2 and CaF2 has efficacy against both brown-rot fungi and white-rot fungus. Similarly, wood treated with the combined NMF formulation is the least susceptible to attack by C. formosanus.It is proposed that combining MgF2 and CaF2changes their overall solubility to promote the release of fluoride ions at the optimal concentration needed for biocidal efficacy against fungi and termites. In this thesis, it was proven that even after leaching, sufficient fluoride was present to protect NMF treated wood from fungal decay. This shows that NMFs are robust enough for above ground contact outdoor applications of wood, where permanent wetness cannot be avoided according to Use Class 3.2, as per the EN 335 (2013) standard. Also, they pose a low risk to human health and the environment because they are sparingly soluble. Since NMFs significantly reduce the decay of wood, the CO2 fixed in it will be retained for longer than in unpreserved wood. Overall, the novel results of this study show the potential of NMFs to increase the service life of building materials made from non-durable wood.
After a general presentation of the beamline, specifically the workflow for ex-situ CT at BAMline is presented. Although being used in a broad variety of research fields the usual workflow for CT experiments is in most cases similar in terms of sample mounting, tomographic scan and reconstruction. Specific scanning schemes allow for a preview reconstruction carried out during the scan. A detailed description of the used hardware as well as the self-coded programs applied in the data pipeline will be given. This will be accompanied by a practical demonstration of the software involved in the entire process.
After a general presentation of the beamline, specifically the workflow for ex-situ CT at BAMline is presented. Although being used in a broad variety of research fields the usual workflow for CT experiments is in most cases similar in terms of sample mounting, tomographic scan and reconstruction. Specific scanning schemes allow for a preview reconstruction carried out during the scan. A detailed description of the used hardware as well as the self-coded programs applied in the data pipeline will be given. This will be accompanied by a practical demonstration of the software involved in the entire process.
The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the data handling pipeline is presented.
We present a workflow for obtaining fully trained artificial neural networks that can perform automatic particle segmentations of agglomerated, non-spherical nanoparticles from scanning electron microscopy images “from scratch”, without the need for large training data sets of manually annotated images. The whole process only requires about 15 minutes of hands-on time by a user and can typically be finished within less than 12 hours when training on a single graphics card (GPU). After training, SEM image analysis can be carried out by the artificial neural network within seconds. This is achieved by using unsupervised learning for most of the training dataset generation, making heavy use of generative adversarial networks and especially unpaired image-to-image translation via cycle-consistent adversarial networks. We compare the segmentation masks obtained with our suggested workflow qualitatively and quantitatively to state-of-the-art methods using various metrics. Finally, we used the segmentation masks for automatically extracting particle size distributions from the SEM images of TiO2 particles, which were in excellent agreement with particle size distributions obtained manually but could be obtained in a fraction of the time.
qNMR provides the most universally applicable form of direct concentration or purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. The workshop presents basic terms of statistics and uncertainty analysis, which are the basis for qNMR spectroscopy and data analysis such as, e.g., standard deviations, linear regression, significance tests, etc. and gives typical examples of applications in qNMR spectroscopy.
The MBLabs consortium comprises various organizations that operate testing facilities encompassing a broad spectrum of tests relevant to the construction sector, particularly building envelopes. In the future, additional testing facilities will join the METABUILDING platform to offer their services. These services will be integrated in the MBLabs Open Innovation Test Bed and accessible via the METABUILDING platform. The METABUILDING platform is operated by the METABUILDING association.
In Task 8.5 the Quality Assurance system of the MBLabs OITB is developed. The presentation gives an overview regarding the development of this system after 3 years of project execution.
Inhibition of respiratory viruses is one of the most urgent topics as underlined by different pandemics in the last two decades. This impels the development of new materials for binding and incapacitation of the viruses. In this work, we have demonstrated that an optimal deployment of influenza A virus (IAV) targeting ligand sialic acid (SA) on a flexible 2D platform enables its binding and wrapping around IAV particles. A series of 2D sialylated platforms consisting graphene and polyglycerol are prepared with different degrees of SA functionalization around 10%, 30%, and 90% named as G-PG-SAL, G-PG-SAM, and G-PG-SAH, respectively. The cryo-electron tomography (Cryo-ET) analysis has proved wrapping of IAV particles by G-PG-SAM.
A confocal-based colocalization assay established for these materials has offered the comparison of binding potential of sialylated and non-sialylated nanoplatforms for IAV. With this method, we have estimated the binding potential of the G-PG-SAM and G-PG-SAH sheets for IAV particles around 50 and 20 times higher than the control sheets, respectively, whereas the low functionalized G-PG-SAL have not shown any significant colocalization value.
Moreover, optimized G-PG-SAM exhibits high potency to block IAV from
binding with the MDCK cells.
The manuscripts – which have been inventoried as Manuscripta Americana in the State Library of Berlin and the Biblioteka Jagellońska in Krakow with the signatures Ms. Americ. 1-15 – are codices mainly from the colonial times of the 16th to 18th centuries. They uniquely reflect the relationships between indigenous culture and Spanish colonial masters. This study focusses on the scientific investigation of three manuscripts (Manuscripta Americana 3, 8, and 10) that are kept today in Krakow. It is assumed that these three parts belong together in a certain way, so various material analyses were carried out to prove this assumption. The scientific investigation focusses on the different black and brown writing inks.
This study focuses on the analysis of a corpus of manuscripts found in Fustat (medieval Cairo, Egypt) in the biggest medieval “archive” found until now: the Cairo Geniza. The giant collection of mostly Jewish documents has been attracting scholars’ attention a lot but so far, the material aspects of these documents seem to have been mainly neglected.
Application of scientific methods of analysis, especially X-Ray fluorescence characterization, contributes to our understanding of the materials used for production of manuscripts during the Middle ages.
Our corpus of the 11th century manuscripts comprises manuscripts written by scribes belonging to three Jewish communities that co-existed in Cairo during this period: the Karaites, the so-called Jerusalemites (or Palestinian) and the so-called Babylonians (or Iraqi), three different communities with different traditions and different leaders. The differences manifest themselves also in the paleographical properties of the manuscripts produced within each community. Can we extend the differences detected by the paleographical analysis to differences in composition of the writing materials and especially the composition of the inks? Or can we relate the differences in the composition to the manuscript type (legal, private...), or to another criterion. In this presentation, we offer answers to some of the questions using statistical analysis of the measurements results.
X-ray back scatter imaging is rarely applied compared to classical X-ray projection imaging. More than 20 years ago the company Philips developed “COMSCAN”, a first application case for aircraft industry, which allowed even a depth resolution using back scatter imaging. The company AS&E in Boston offers back scatter imaging solutions for the security market. The principle is to scan the object with a highly collimated X-ray needle beam from one side only and to detect the backscattered radiation by a large area detector side by side with the collimation wheel. A new prototype is investigated at BAM for application and optimization in non-destructive testing. As modern industrial application field in-situ inspection in additive manufacturing is targeted. The accessibility of the printed part during the production process is very limited. This prevent the application of a two sided X-ray inspection or Computed Tomography, were an rotation of the object is required to acquire projections from 360 degrees. An important advantage for the X-ray back scatter technique are also the materials used in additive manufacturing (polymers, ceramics, light metals like Aluminum or Titanium). These materials with lower density and lower Z values give better scatter signals than metals with higher densities and Z values. The back scatter intensity decreases with increasing density and Z value of the material. But the requirements on spatial resolution and contrast sensitivity are more stringent for non-destructive testing of additive manufactured parts compared to the security area. In NDT sizes of indications smaller than 1 mm have to be detected clearly. The investigation of these limits on a state-of-the-art prototype for X-ray back scattering using rotating collimated X-ray needle beams is a part of the BAM project “ProMoAM”. The contribution shows first results of the optimization for NDT and the achieved application limits for several example cases.
X-ray back scatter imaging is rarely applied compared to classical X-ray projection imaging. 20 years ago the company Philips developed “COMSCAN”, a first application case in the aircraft industry, which allowed even a depth resolution using back scatter imaging. The company AS&E in Boston offers back scatter imaging solutions for the security market. Their principle is to scan the object with a highly collimated X-ray needle beam from one side only and detect the backscattered radiation by a large area detector side by side with the collimation wheel. A new prototype is investigated at BAM for application and optimization in non-destructive testing. As modern industrial application field in-situ testing in additive manufacturing is targeted. The accessibility of the printed part during the production process is very limited. This prevent the application of a two sided X-ray inspection or Computed Tomography, were an rotation of the object is required to acquire projections from 360 degrees. An important advantage for the X-ray back scatter technique are also the materials used in additive manufacturing (polymers, ceramics, light metals like Aluminum or Titanium). These materials with lower density and lower Z values give better scatter signals than metals with higher densities and Z values. The back scatter intensity decreases with increasing density and Z value of the material. But the requirements on spatial resolution and contrast sensitivity are more stringent for non-destructive testing of additive manufactured parts compared to the security area. In NDT sizes of indications smaller than 1 mm have to be detected clearly. The investigation of these limits on a stateof-the-art prototype for X-ray back scattering using rotating collimated X-ray needle beams is a part of the BAM project “ProMoAM”. The contribution shows first results of the optimization for NDT and the achieved application limits for several example cases.
X-ray back scatter imaging is rarely applied compared to classical X-ray projection imaging. 20 years ago the company Philips developed “COMSCAN”, a first application case in the aircraft industry, which allowed even a depth resolution using back scatter imaging. The company AS&E in Boston offers back scatter imaging solutions for the security market. Their principle is to scan the object with a highly collimated X-ray needle beam from one side only and detect the backscattered radiation by a large area detector side by side with the collimation wheel. A new prototype is investigated at BAM for application and optimization in non-destructive testing. As modern industrial application field in-situ testing in additive manufacturing is targeted. The accessibility of the printed part during the production process is very limited. This prevent the application of a two sided X-ray inspection or Computed Tomography, were an rotation of the object is required to acquire projections from 360 degrees. An important advantage for the X-ray back scatter technique are also the materials used in additive manufacturing (polymers, ceramics, light metals like Aluminum or Titanium). These materials with lower density and lower Z values give better scatter signals than metals with higher densities and Z values. The back scatter intensity decreases with increasing density and Z value of the material. But the requirements on spatial resolution and contrast sensitivity are more stringent for non-destructive testing of additive manufactured parts compared to the security area. In NDT sizes of indications smaller than 1 mm have to be detected clearly. The investigation of these limits on a stateof-the-art prototype for X-ray back scattering using rotating collimated X-ray needle beams is a part of the BAM project “ProMoAM”. The contribution shows first results of the optimization for NDT and the achieved application limits for several example cases.
Additively manufactured (AM) metallic sheet-based Triply Periodic Minimal Surface Structures (TPMSS) meet several requirements in both bio-medical and engineering fields: Tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some challenges related to quality control, which can prevent their successful application. In fact, the optimization of the AM process is impossible without considering structural characteristics as manufacturing accuracy, internal defects, as well as surface topography and roughness. In this study, the quantitative non-destructive analysis of TPMSS manufactured from Ti-6Al-4V alloy by electron beam melting was performed by means of X-ray computed tomography (XCT). Several advanced image analysis workflows are presented to evaluate the effect of build orientation on wall thicknesses distribution, wall degradation, and surface roughness reduction due to the chemical etching of TPMSS. It is shown that the manufacturing accuracy differs for the structural elements printed parallel and orthogonal to the manufactured layers. Different strategies for chemical etching show different powder removal capabilities and both lead to the loss of material and hence the gradient of the wall thickness. This affects the mechanical performance under compression by reduction of the yield stress. The positive effect of the chemical etching is the reduction of the surface roughness, which can potentially improve the fatigue properties of the components. Finally, XCT was used to correlate the amount of retained powder with the pore size of the functionally graded TPMSS, which can further improve the manufacturing process.
This study focuses on the analysis of a corpus of manuscripts found in Fustat (medieval Cairo, Egypt) in the biggest medieval “archive” found until now: the Cairo Geniza. The giant collection of mostly Jewish documents has been attracting scholars’ attention a lot but so far, the material aspects of these documents seem to have been mainly neglected.
Application of scientific methods of analysis, especially X-Ray fluorescence characterization, contributes to our understanding of the materials used for production of manuscripts during the Middle ages.
Our corpus of the 11th century manuscripts comprises manuscripts written by scribes belonging to three Jewish communities that co-existed in Cairo during this period: the Karaites, the so-called Jerusalemites (or Palestinian) and the so-called Babylonians (or Iraqi), three different communities with different traditions and different leaders. The differences manifest themselves also in the paleographical properties of the manuscripts produced within each community. Can we extend the differences detected by the paleographical analysis to differences in composition of the writing materials and especially the composition of the inks? Or can we relate the differences in the composition to the manuscript type (legal, private...), or to another criterion. In this presentation, we offer answers to some of the questions using statistical analysis of the measurements results.
Our aim is to develop a new simple and inexpensive method for full field X-ray fluorescence imaging . We combine an energy dispersive array detector with a coded aperture to obtain high resolution images . To obtain the information from the recorded image a reconstruction step is necessary . The reconstruction methods we have developed , were tested on simulated data and then applied to experimental data . The first tests were carried out at the BAM line @ BESSY II. This method enables the simultaneous detection of multiple elements , which is important e.g. in the field of catalysis.
Our aim is to develop a new method for full field X ray fluorescence imaging at the BAM line @ BESSY II. We will combine an energydispersive array detector for X rays with a coded aperture to get high resolution images . In coded aperture imaging , an object is projected through a mask , producing many overlapping images on the detector . The first part of the project is to perform raytracing simulations to get realistic data and to develop a reconstruction method that allows to get the Information about the investigated object out of the projected image .
We developed a new method for full field X-ray fluorescence imaging at the BAMline @ BESSY II. We combined an energy dispersive array detector for X-rays with a coded aperture to get high resolution images.
In coded aperture imaging, an object is projected through a mask, producing many overlapping images on the detector. To get the information about the investigated object out of the projected image, a decoding step is necessary.
The first part of our project was to develop the decoding algorithms. We tested the reported reconstruction with an antimask and compared the results with the performance of self-written reconstruction programs based on an iterative and a genetic algorithm. First tests were performed with raytracing simulations.
The next step was the collection of experimental data at the BAMline @ BESSY II (HZB). A test objects could be successfully reconstructed with our newly developed algorithm.
In this talk, the features of X-ray fluorescence analysis with synchrotron radiation will be presented. First, the basics of the origin of synchrotron radiation and X-ray fluorescence analysis and the experimental setup will be discussed. Then, examples of trace element detection, micrometer resolution, and application of the X-ray color camera will be shown.
X-ray generation
(2020)
The literature has shown that the application of laminography provides advantages as 3D radiographic imaging with depth information for in house and mobile testing. This permits to distinguish between overlapping indications, measure the extension along radiation direction and classify indications as surface open or subsurface
ones as required in critical engineering assessment. This work provides a comparative study and measurements of the three techniques Digital Radiography (DR) with Digital Detector Arrays (DDA), Coplanar Translational Laminography (CTL) and Computed Tomography (CT), applied for composite pipeline inspection. It is demonstrated that CTL and CT provide advantages for the evaluation of pipe-to-pipe connections and the evaluation of adhesive applications. They show indications of discontinuities with higher contrast sensitivity than radiography.
Beyond it, two specimen, namely Phantom 1 and Phantom 2, were developed and manufactured by additive manufacturing to analyze the preferential detection sensitivity and the direction of features and depth information for laminographic measurements. Another goal was to show the laminographic capabilities to distinguish between overlapping discontinuities. CTL is especially suitable for mobile inspection. Special glass fiber reinforced polymer samples (GRP) were manufactured for further analysis and comparisons between the abovementioned techniques. Finally, Phantoms 1 and 2 show the capability of laminography to detect overlapping indications and also show that discontinuities oriented perpendicular to the scan direction have the highest contrast sensitivity for laminographic measurements.
Functional materials for energy conversion are important technology drivers needed for the implementation of low carbon energy. Therefore, researchers commonly focus on improving the intrinsic properties of a functional material. However, for applications, the extrinsic properties are at least as important as the intrinsic ones. Consequently, it is important to investigate and understand the external and internal structure of semi-finished products and especially defect dependent properties. The extrinsic properties may change during application and the life cycle of the material as well as through processing and molding steps. Our studies show how X-ray tomographic (XCT) investigations can contribute to structure investigations in composites and massive samples using the example of magnetic materials for energy conversion.
Heterogeneous catalysis is a key technology in modern industrial societies. The main steps of a catalytic process take place at the surfaces of complex materials. For the investigations of these surfaces X-ray photoelectron spectroscopy is widely used and fits ideally. At some suitable examples, it will be explained how XPS can help to understand such catalysts better. The focus is on selective oxidation catalysts, one of the main challenges of present research. Here it will illustrate, how changes in the near surface region influence the catalyst performance and, herewith the different stages (activation, maximum performance and deactivation) in the life of catalysts. Additionally, it will be stressed out how important information at different depth regions (surface, near-surface region, bulk) can be useful for comprehensive understanding of the material.
Another important subject is nanostructured catalysts with molecular sieves as supports or defined complexes as precursors. Finally, the combination of XPS with other methods used in the analysis of catalysts, e.g. electron microscopy, X-ray absorption spectroscopy and low energy ion scattering will be discussed.
X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). Importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks and quantify their densities in bulk (not too heavy) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, they can detect objects with size above a few wavelengths of the radiation.
Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads.
The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models.
We hereby show the application of non-destructive X-ray refraction radiography (SXRR, 2D mapping also called topography) to problems in additive manufacturing:
1) Porosity analysis in PBF-LM-Ti64. Through the use of SXRR, we could not only map the (very sparse) porosity distribution between the layers and quantify it, but also classify, and thereby separate, the filled porosity (unmolten powder) from the keyhole and gas pores (Figure 1).
2) In-situ heat treatment of laser powder bed fusion PBF-LM-AlSi10Mg to monitor microstructure and porosity evolution as a function of temperature (Figure 2). By means of SXRR we indirectly observed the initial eutectic Si network break down into larger particles as a function of increasing temperature. We also could detect the thermally induced porosity (TIP). Such changes in the Si-phase morphology upon heating is currently only possible using scanning electron microscopy, but with a much smaller field-of-view. SXRR also allows observing the growth of some individual pores, usually studied via X-ray computed tomography, but again on much smaller fields-of-view.
Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the defect distribution and the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes.
For the first time, X-ray refraction techniques are proven for the identification of void formation in Ti-6Al-4V parts produced by selective laser melting. The topology and volume fraction of pores are measured in samples produced with different laser energy density. Unique X-ray refraction methods identify different kinds of defects, characteristic to the regions below and above the Optimum laser energy density, namely unprocessed powder (unmolten powder particles, balling effect, and Fusion defects) from empty keyhole pores. Furthermore, it is possible to detect small inhomogeneities (voids or cracks) with sizes below the spatial resolution of optical microscopy and X-ray computed tomography.
This dataset contains the processed and analysed small-angle X-ray scattering data associated with all samples from the publications "Bio-SAXS of Single-Stranded DNA-Binding Proteins: Radiation Protection by the Compatible Solute Ectoine" (https://doi.org/10.1039/D2CP05053F).
Files associated with McSAS3 analyses are included, alongside the relevant SAXS data, with datasets labelled in accordance to the protein (G5P), its concentration (1, 2 or 4 mg/mL), and if Ectoine is present (Ect) or absent (Pure). PEPSIsaxs simulations of the GVP monomer (PDB structure: 1GV5 ) and dimer are also included.
TOPAS-bioSAXS-dosimetry extension for TOPAS-nBio based particle scattering simulations can be obtained from https://github.com/MarcBHahn/TOPAS-bioSAXS-dosimetry which is further described in https://doi.org/10.26272/opus4-55751.
This work was funded by the Deutsche Forschungsgemeinschaft (DFG, German Research Foundation) under grant number 442240902 (HA 8528/2-1 and SE 2999/2-1). We acknowledge Diamond Light Source for time on Beamline B21 under Proposal SM29806. This work has been supported by iNEXT-Discovery, grant number 871037, funded by the Horizon 2020 program of the European Commission.
X-ray scattering datasets for samples described in the 2020 publication "Molecular Dynamics of Janus Polynorbornenes: Glass Transitions and Nanophase Separation". This dataset includes both raw and processed X-ray scattering data for samples PTCHSiO-Pr, Bu, Hx, Oc and De, alongside background measurements files (BKG). This data was collected using the MOUSE project (instrument and methodology).
X-ray scattering datasets for samples described in the 2022 publication "Molecular Mobility of Polynorbornenes with Trimethylsiloxysilyl side groups: Influence of the Polymerization Mechanism". This dataset includes both raw and processed X-ray scattering data for samples APTCN and MPTCN, alongside background measurements files (BKG).
X-ray scattering datasets for samples described in the 2022 publication "Side chain length dependent dynamics and conductivity in self assembled ion channels". This dataset includes both raw and processed X-ray scattering data for samples ILC8, ILC10, ILC12, ILC14 and ILC16 alongside background measurement files (BKG).
Wide-range X-ray scattering datasets and analyses for all samples described in the 2020 publication "Gold and silver dichroic nanocomposite in the quest for 3D printing the Lycurgus cup". These datasets are composed by combining multiple small-angle x-ray scattering and wide-angle x-ray scattering curves into a single dataset. They have been analyzed using McSAS to extract polydispersities and volume fractions. They have been collected using the MOUSE project (instrument and methodology).
Compared to the clear, real-space images you can get from electron microscopy, X-ray scattering patterns are rather featureless. These patterns, however, contain structural information from all of the material structure illuminated by the X-ray beam. With this technique, you can measure nanoparticle dispersions, catalysts, composites, MOF powders, battery materials, light metal alloys and gels to reveal information on the structural features found within these materials. We have even measured many such materials for several research groups from the University of Birmingham, revealing structure features in the sub-nm to the micrometer range.
Measuring an X-ray scattering pattern is relatively easy, but measuring a high-quality, useful pattern requires significant effort and good laboratory organization. Such laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration) [1]. With the MOUSE, we have combined: a) a comprehensive and highly automated laboratory workflow with b) a heavily modified X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, within a well-documented, FAIR-compliant data flow (akin to what is found at the more automated synchrotron beamlines). With two full-time researchers, our lab collects and interprets thousands of datasets, on hundreds of samples, for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data.
Measuring an X-ray scattering pattern is relatively easy, but measuring a steady stream of high-quality, useful patterns requires significant effort and good laboratory organization.
Such laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration).
With the MOUSE, we have combined a comprehensive and highly automated laboratory workflow with a heavily modified X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, within a well-documented, FAIR-compliant data flow (akin to what is found at the more automated synchrotron beamlines). With two full-time researchers, our lab collects and interprets thousands of datasets, on hundreds of samples, for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data.
This talk will briefly introduce the foundations of X-ray scattering, present the MOUSE project, and will highlight the proven utility of the methodology for materials science. Upgrades to the methodology will also be discussed, as well as possible avenues for transferring this holistic methodology to other instruments
X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks and quantify their densities in bulk (not too heavy) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation.
We thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in materials science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in additively manufactured alloys; 3) Fiber de-bonding in metal and polymer matrix composites.
Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads. Applications of in-situ X-ray refraction radiography on aluminum alloys and composites are also shown.
The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models.
X-rays without X-rays: Can muon tomography provide pictures from within concrete and other objects?
(2024)
Until the 1980s radiography was used to inspect civil structures in case of special demands and showed a much better resolution than other NDT techniques. However, due to safety concerns and cost issues, this method is almost never used anymore. Meanwhile, non-destructive techniques such as ultrasound or
radar have found regular, successful practical application but sometimes suffer from limited resolution and accuracy, imaging artefacts or restrictions in detecting certain features when applied to reinforced or prestressed concrete inspection.
Muon tomography has received much attention recently. Muons are particles generated naturally by cosmic rays in the upper atmosphere and pose no risk to humans. Novel detectors and tomographic imaging algorithms have opened new fields of application, mainly in the nuclear sector, but also in spectacular cases such as the Egyptian pyramids.
As a first step towards practical application in civil engineering and as a proof of concept we used an existing system to image the interior of a reference reinforced 600 kg concrete block. Even with a yet not optimized setup for this kind of investigation, the muon imaging results have been at least of similar quality compared to ultrasonic and radar imaging, potentially even better. Recently, the research was expanded to more realistic testing problems such as the detection of voids in certain structural elements. However, before practical implementation, more robust, mobile, and affordable detectors would be required as well as user-Friendly imaging and simulation software.
The talk also discusses other applications , such as volcanology, mining and geothermal exploration.