Laboratory-based X-ray Source Research Articles

Determining pair distribution functions of thin films using laboratory-based X-ray sources

Determining pair distribution functions of thin films using laboratory-based X-ray sources

Challenges in non-destructive X-ray CT testing of riveted joints in the automotive industry

Despite recent advancements, contemporary laboratory-based industrial computed tomography (CT) technology has not yet achieved the status of an efficient and economically viable in situ non-destructive method for examining riveted joints that are commonly used in the automotive industry. 2D X-ray or 3D CT systems can only reliably assess a rivet joint’s condition in rare, and favorable circumstances. Moreover, a comprehensive analysis to identify the obstacles preventing CT from efficiently capturing high-resolution, and contrast-rich scans of riveted joints in general is lacking. This work delves into the challenges and limitations of the technology that prevent operators from reaching the desired precision required for rigorous quality control. The study specifically addresses questions concerning in situ reachability and positioning of the sample structure, radiodensity and beam hardening, the relationship between spot size and power, and economic feasibility—all within the context of analyzing riveted joints in the automotive industry. Additionally, we provide an abstracted overview of the current industrial X-ray tube market, which informs our discussion on these specific aspects. Through a combination of experimental findings, analytical insights, and deductions, we shed light on the persistent difficulties in achieving resolutions comparable to macro-sectioning and microscopy, which are currently considered the gold standard in examining riveted joints. Our investigation further explores the potential of a photon-counting detector paired with a conventional, laboratory-based X-ray source. Furthermore, we investigate the use of a synchrotron beamline as an X-ray source in conjunction with a custom-designed detector optimized for such beam geometries. This detector employs scintillators coupled with optical magnification, functioning similarly to an X-ray microscope. Our findings and data collection conclusively reveal that commercially available CT systems still fail to meet the requirements for efficient testing, underscoring the urgent need for further research and development to enable widespread implementation.

Flash X-ray radiography of internal damage in soft cellular materials during instrumented dynamic penetration

Processes of internal damage development during localized dynamic penetration represent a crucial mechanism important for relevant analysis of deformation and failure of plates and sandwich panels under high strain rate conditions. Soft cellular materials are of special importance as the internal damage defines mode of collapse and energy absorption capabilities. In this paper, a fast X-ray radiography is employed for in-situ analysis of the internal damage development in soft closed-cell aluminum foam subjected to a localized high strain rate penetration using an instrumented projectile in a direct impact Hopkinson bar apparatus. The process with a typical duration of a few milliseconds is visualized using four X-ray projections acquired using a flash X-ray system and a high-speed camera. Internal damage such as cracking, shear failure in the vicinity of the projectile, and compaction of the material is successfully identified. This unique method utilizing a laboratory based X-ray source allows for characterization of the penetration mechanism that has been usually analyzed only in post-mortem state.

The intensity enhancement of transmission small angle x-ray scattering from nanostructures with a high aspect ratio

Transmission small angle x-ray scattering (tSAXS) has been developed as a metrology for the critical dimension (CD) measurements to facilitate integrated circuit (IC) chip fabrications. Synchrotron x-ray sources were used for their high brilliance and a wavelength less than one tenth of a nanometer was chosen for its high penetration power to enable transmission measurements through a silicon wafer with a nominal thickness of 0.7 mm. A major hold back preventing tSAXS from reaching wide applications in IC fabrication is the lack of high brilliance laboratory-based x-ray sources. Within the last few years, even without any major breakthrough in x-ray source technology, this tSAXS metrology has finally been used for 3D NAND and DRAM, i.e., memory chips with tall or high aspect ratio (HAR) architectures. The scattering intensities from HAR structures will be discussed quantitatively in terms of the sample height and the effective longitudinal coherence length of the incident x-ray.

In situ x-ray computed tomography of zinc–air primary cells during discharge: correlating discharge rate to anode morphology

Zinc–air batteries have gained significant attention as safe battery alternatives, with high theoretical energy densities and a high abundance of their constituent materials. However, barriers to their widespread adoption include the need to improve their cycling lifetime, as well as stability and avoiding degradation mechanisms such as zinc dendrite growth and hydrogen-producing side reactions. X-ray computed tomography (CT) is a widely used technique for the study of batteries. In situ / operando x-ray CT has been increasingly used to study the zinc anode of zinc–air batteries to evaluate the interesting morphological changes occurring during the reaction from zinc (Zn) to zinc oxide (ZnO) during discharge (vice versa during charge). However, several studies have been carried out using synchrotron x-ray sources, which have limited availability for users. In this work, we present a comprehensive study of the discharge of commercial, primary zinc–air batteries using a laboratory-based x-ray source for in situ x-ray CT measurements. Four different discharge rates are investigated (C/30, C/60, C/90 and C/150), with tomograms collected at various stages throughout each discharge. Results confirm that with decreasing C-rate (i.e. decreasing discharge current) a greater volume of zinc is reacted, with average mass utilisations of 17%, 76%, 81% and 87% for C/30, C/60, C/90 and C/150, respectively. Furthermore, quantification using x-ray CT datasets showed that there is a direct correlation between the volume of zinc remaining in the cell and the state-of-charge of the cell, which deviated from linearity for the longer C-rates. Finally, a potential new mechanism for shape change is discussed, where a Zn particle is replaced with a pore of a similar volume. As well as improvements in statistical relevance gained from multiple repeats for each C-rate, the results presented here could be used in both modelling of battery performance, as well as consideration for future anode design concepts.

Optimizing laboratory X-ray diffraction contrast tomography for grain structure characterization of pure iron.

Laboratory diffraction contrast tomography (LabDCT) is a recently developed technique for 3D nondestructive grain mapping using a conical polychromatic beam from a laboratory-based X-ray source. The effects of experimental parameters, including accelerating voltage, exposure time and number of projections used for reconstruction, on the characterization of the 3D grain structure in an iron sample are quantified. The experiments were conducted using a commercial X-ray tomography system, ZEISS Xradia 520 Versa, equipped with a LabDCT module; and the data analysis was performed using the software package GrainMapper3D, which produces a 3D reconstruction from binarized 2D diffraction patterns. It is found that the exposure time directly affects the background noise level and thus the ability to distinguish weak spots of small grains from the background. With the assistance of forward simulations, it is found that spots from the first three strongest {hkl} families of a large grain can be seen with as few as 30-40 projections, which is sufficient for indexing the crystallographic orientation and resolving the grain shape with a reasonably high accuracy. It is also shown that the electron current is a more important factor than the accelerating voltage to be considered for optimizing the photon numbers with energies in the range of 20-60 keV. This energy range is the most important one for diffraction of common metals, e.g. iron and aluminium. Several suggestions for optimizing LabDCT experiments and 3D volume reconstruction are finally provided.

Ptychographic X-ray speckle tracking with multi-layer Laue lens systems.

The ever-increasing brightness of synchrotron radiation sources demands improved X-ray optics to utilize their capability for imaging and probing biological cells, nano-devices and functional matter on the nanometre scale with chemical sensitivity. Hard X-rays are ideal for high-resolution imaging and spectroscopic applications owing to their short wavelength, high penetrating power and chemical sensitivity. The penetrating power that makes X-rays useful for imaging also makes focusing them technologically challenging. Recent developments in layer deposition techniques have enabled the fabrication of a series of highly focusing X-ray lenses, known as wedged multi-layer Laue lenses. Improvements to the lens design and fabrication technique demand an accurate, robust, in situ and at-wavelength characterization method. To this end, a modified form of the speckle tracking wavefront metrology method has been developed. The ptychographic X-ray speckle tracking method is capable of operating with highly divergent wavefields. A useful by-product of this method is that it also provides high-resolution and aberration-free projection images of extended specimens. Three separate experiments using this method are reported, where the ray path angles have been resolved to within 4 nrad with an imaging resolution of 45 nm (full period). This method does not require a high degree of coherence, making it suitable for laboratory-based X-ray sources. Likewise, it is robust to errors in the registered sample positions, making it suitable for X-ray free-electron laser facilities, where beam-pointing fluctuations can be problematic for wavefront metrology.

Ptychographic X-ray speckle tracking.

A method is presented for the measurement of the phase gradient of a wavefront by tracking the relative motion of speckles in projection holograms as a sample is scanned across the wavefront. By removing the need to obtain an undistorted reference image of the sample, this method is suitable for the metrology of highly divergent wavefields. Such wavefields allow for large magnification factors that, according to current imaging capabilities, will allow for nanoradian angular sensitivity and nanoscale sample projection imaging. Both the reconstruction algorithm and the imaging geometry are nearly identical to that of ptychography, except that the sample is placed downstream of the beam focus and that no coherent propagation is explicitly accounted for. Like other X-ray speckle tracking methods, it is robust to low-coherence X-ray sources, making it suitable for laboratory-based X-ray sources. Likewise, it is robust to errors in the registered sample positions, making it suitable for X-ray free-electron laser facilities, where beam-pointing fluctuations can be problematic for wavefront metrology. A modified form of the speckle tracking approximation is also presented, based on a second-order local expansion of the Fresnel integral. This result extends the validity of the speckle tracking approximation and may be useful for similar approaches in the field.

A partial-dithering strategy for edge-illumination x-ray phase-contrast tomography enabled by a joint reconstruction method

Edge-illumination x-ray phase-contrast tomography (EIXPCT) is a promising imaging technology where partially opaque masks are utilized with laboratory-based x-ray sources to estimate the distribution of the complex-valued refractive index. EIXPCT resolution is mainly determined by the period of a sample mask, but can be significantly improved by a dithering technique. Here, dithering means that multiple images per tomographic view angle are acquired as the object is moved over sub-pixel distances. Drawbacks of dithering include increased data-acquisition times and radiation doses. Motivated by the flexibility in data-acquisition designs enabled by a recently developed joint reconstruction method, a novel partial-dithering strategy for EIXPCT data-acquisition is proposed. In this strategy, dithering is implemented at only a subset of the tomographic view angles. The strategy can result in spatial resolution comparable to that of the conventional full-dithering strategy, where dithering is performed at every view angle, but the acquisition time is substantially decreased. Here, the effect of dithering parameters on image resolution is explored.

Comparison of data-acquisition designs for single-shot edge-illumination X-ray phase-contrast tomography.

Edge-illumination X-ray phase-contrast tomography (EIXPCT) is an emerging technique that enables practical phase-contrast imaging with laboratory-based X-ray sources. A joint reconstruction method was proposed for reconstructing EIXPCT images, enabling novel flexible data-acquisition designs. However, only limited efforts have been devoted to optimizing data-acquisition designs for use with the joint reconstruction method. In this study, several promising designs are introduced, such as the constant aperture position (CAP) strategy and the alternating aperture position (AAP) strategy covering different angular ranges. In computer-simulation studies, these designs are analyzed and compared. Experimental data are employed to test the designs in real-world applications. All candidate designs are also compared for their implementation complexity. The tradeoff between data-acquisition time and image quality is discussed.

Visualizing treatment delivery and deposition in mouse lungs using in vivo x-ray imaging

The complexity of lung diseases makes pre-clinical in vivo respiratory research in mouse lungs of great importance for a better understanding of physiology and therapeutic effects. Synchrotron-based imaging has been successfully applied to lung research studies, however longitudinal studies can be difficult to perform due to limited facility access. Laboratory-based x-ray sources, such as inverse Compton x-ray sources, remove this access limitation and opens up new possibilities for pre-clinical small-animal lung research at high spatial and temporal resolution. The in vivo visualization of drug deposition in mouse lungs is of interest, particularly in longitudinal research, because the therapeutic outcome is not only dependent on the delivered dose of the drug, but also on the spatial distribution of the drug. An additional advantage of this approach, when compared to other imaging techniques, is that anatomic and dynamic information is collected simultaneously. Here we report the use of dynamic x-ray phase-contrast imaging to observe pulmonary drug delivery via liquid instillation, and by inhalation of micro-droplets. Different liquid volumes (4 μl, 20 μl, 50 μl) were tested and a range of localized and global distributions were observed with a temporal resolution of up to 1.5 fps. The in vivo imaging results were confirmed by ex vivo x-ray and fluorescence imaging. This ability to visualize pulmonary substance deposition in live small animals has provided a better understanding of the two key methods of delivery; instillation and nebulization.

Photon flux determination of a liquid-metal jet X-ray source by means of photon scattering

Liquid-metal jet X-ray sources promise to deliver high photon fluxes, which are unprecedented for laboratory based X-ray sources, because the regenerating liquid-metal anode is less sensitive to damage caused by an increased electron beam power density.

Implementation of a Computed Tomography System based on a laboratory-based nanofocus X-ray source.

Implementation of a Computed Tomography System based on a laboratory-based nanofocus X-ray source.

Laboratory-scale X-ray absorption spectroscopy approach for actinide research: Experiment at the uranium L3-edge

We report that by using crystal optics and laboratory-based X-ray source, one may perform easily X-ray Absorption Spectroscopy (XAS) state-of-the-art measurements at the U L3-edge. Our results are in excellent agreement with synchrotron-based studies for UO2, KUO3 and β-UO3. The laboratory scaled approach constitutes an inexpensive solution to the limited availability of the XAS beamlines for actinide research. Moreover, our results allow for the development of many future applications addressing actinide f-electron chemistry and nuclear energy-related physico-chemistry, such as advanced nuclear fuel development and safe long term disposal of nuclear wastes.

Phase-and-amplitude recovery from a single phase-contrast image using partially spatially coherent x-ray radiation

A simple method of phase-and-amplitude extraction is derived that corrects for image blurring induced by partially spatially coherent incident illumination using only a single intensity image as input. The method is based on Fresnel diffraction theory for the case of high Fresnel number, merged with the space-frequency description formalism used to quantify partially coherent fields and assumes the object under study is composed of a single-material. A priori knowledge of the object’s complex refractive index and information obtained by characterizing the spatial coherence of the source is required. The algorithm was applied to propagation-based phase-contrast data measured with a laboratory-based micro-focus x-ray source. The blurring due to the finite spatial extent of the source is embedded within the algorithm as a simple correction term to the so-called Paganin algorithm and is also numerically stable in the presence of noise.

Myoanatomy of the velvet worm leg revealed by laboratory-based nanofocus X-ray source tomography

X-ray computed tomography (CT) is a powerful noninvasive technique for investigating the inner structure of objects and organisms. However, the resolution of laboratory CT systems is typically limited to the micrometer range. In this paper, we present a table-top nanoCT system in conjunction with standard processing tools that is able to routinely reach resolutions down to 100 nm without using X-ray optics. We demonstrate its potential for biological investigations by imaging a walking appendage of Euperipatoides rowelli, a representative of Onychophora-an invertebrate group pivotal for understanding animal evolution. Comparative analyses proved that the nanoCT can depict the external morphology of the limb with an image quality similar to scanning electron microscopy, while simultaneously visualizing internal muscular structures at higher resolutions than confocal laser scanning microscopy. The obtained nanoCT data revealed hitherto unknown aspects of the onychophoran limb musculature, enabling the 3D reconstruction of individual muscle fibers, which was previously impossible using any laboratory-based imaging technique.

Laboratory-based X-ray phase-imaging scanner using Talbot-Lau interferometer for non-destructive testing

An X-ray Talbot-Lau interferometer scanning setup consisting of three transmission gratings, a laboratory-based X-ray source that emits X-rays vertically, and an image detector on the top has been developed for the application of X-ray phase imaging to moving objects that cannot be tested clearly with conventional absorption contrast. The grating-based X-ray phase imaging method usually employs a phase-stepping (or fringe-scanning) technique by displacing one of the gratings step-by-step while the object stays still. Since this approach is not compatible with a scanner-type application for moving objects, we have developed a new algorithm for achieving the function of phase-stepping without grating displacement. By analyzing the movie of the moiré pattern as the object moves across the field of view, we obtain the absorption, differential phase, and visibility images. The feasibility of the X-ray phase imaging scanner has been successfully demonstrated for a long sample moving at 5 mm/s. This achievement is a breakthrough for the practical industrial application of X-ray phase imaging for screening objects carried on belt-conveyers such as those in factories.

An iterative method for near-field Fresnel region polychromatic phase contrast imaging

We present an iterative method for polychromatic phase contrast imaging that is suitable for broadband illumination and which allows for the quantitative determination of the thickness of an object given the refractive index of the sample material. Experimental and simulation results suggest the iterative method provides comparable image quality and quantitative object thickness determination when compared to the analytical polychromatic transport of intensity and contrast transfer function methods. The ability of the iterative method to work over a wider range of experimental conditions means the iterative method is a suitable candidate for use with polychromatic illumination and may deliver more utility for laboratory-based x-ray sources, which typically have a broad spectrum.

Elemental Contrast X-ray Tomography Using Ross Filter Pairs with a Polychromatic Laboratory Source

The majority of current laboratory based X-ray sources are polychromatic and are not tuneable. This lack of monochromaticity limits the range of applications for these sources and in particular it reduces the elemental specificity of laboratory based X-ray imaging experiments. Here we present a solution to this problem based on the use of Ross filter pairs. Although such Ross filter arrangements have been applied in proof-of-principle spectroscopy experiments, to date there have been no reports of this approach used for full-field X-ray imaging. Here we report on the experimental demonstration of Ross filter pairs being used for quasi-monochromatic, full-field imaging. This arrangement has several important benefits for laboratory based X-ray imaging including, as we demonstrate, elemental contrast enhancement. The method is demonstrated both for two-dimensional radiography and for three-dimensional X-ray tomography.

Energy-windowed, pixellated X-ray diffraction using the Pixirad CdTe detector

X-ray diffraction (XRD) is a powerful tool for material identification. In order to interpret XRD data, knowledge is required of the scattering angles and energies of X-rays which interact with the sample. By using a pixellated, energy-resolving detector, this knowledge can be gained when using a spectrum of unfiltered X-rays, and without the need to collimate the scattered radiation. Here we present results of XRD measurements taken with the Pixirad detector and a laboratory-based X-ray source. The cadmium telluride sensor allows energy windows to be selected, and the 62 μm pixel pitch enables accurate spatial information to be preserved for XRD measurements, in addition to the ability to take high resolution radiographic images. Diffraction data are presented for a variety of samples to demonstrate the capability of the technique for materials discrimination in laboratory, security and pharmaceutical environments. Distinct diffraction patterns were obtained, from which details on the molecular structures of the items under study were determined.