Implementation of grain mapping by diffraction contrast tomography on a conventional laboratory tomography setup with various detectors.

Laboratory-based diffraction contrast tomography (LabDCT) is a novel technique used to resolve grain orientations and shapes in three dimensions at the micrometre scale using laboratory X-ray sources, allowing the user to overcome the constraint of limited access to synchrotron facilities. To foster the development of this technique, the implementation of LabDCT is illustrated in detail using a conventional laboratory-based X-ray tomography setup, and it is shown that such implementation is possible with the two most common types of detectors: CCD and flat panel. As a benchmark, LabDCT projections were acquired on an AlCu alloy sample using the two types of detectors at different exposure times. Grain maps were subsequently reconstructed using the open-source grain reconstruction method reported in the authors' previous work. To characterize the detection limit and the spatial resolution for the current implementation, the reconstructed LabDCT grain maps were compared with the map obtained from a synchrotron measurement, which is considered as ground truth. The results show that the final grain maps from measurements by the CCD and flat panel detector are similar and show comparable quality, while the CCD gives a much better contrast-to-noise ratio than the flat panel. The analysis of the grain maps reconstructed from measurements with different exposure times suggests that a grain map of comparable quality could be obtained in less than 1 h total acquisition time without a significant loss of grain reconstruction quality and indicates a clear potential for time-lapse LabDCT experiments. The current implementation is suggested to promote the generic use of the LabDCT technique for grain mapping on conventional tomography setups.

Reconstruction algorithms for grain mapping by laboratory X-ray diffraction contrast tomography.

X-ray-based non-destructive 3D grain mapping techniques are well established at synchrotron facilities. To facilitate everyday access to grain mapping instruments, laboratory diffraction contrast tomography (LabDCT), using a laboratory-based conical polychromatic X-ray beam, has been developed and commercialized. Yet the currently available LabDCT grain reconstruction methods are either ill-suited for handling a large number of grains or require a commercial licence bound to a specific instrument. To promote the availability of LabDCT, grain reconstruction methods have been developed with multiple reconstruction algorithms based on both forward and back calculations. The different algorithms are presented in detail and their efficient implementation using parallel computing is described. The performance of different reconstruction methods is assessed on synthetic data. The code to implement all the described algorithms has been made publicly accessible with the intention of fostering the development of grain mapping techniques on widely available laboratory instruments.

Miniature laser powder bed fusion system for in situ synchrotron x-ray micro-computed tomography experiments at the European Synchrotron Radiation Facility.

We describe our miniature laser powder bed fusion (L-PBF) system for in situ synchrotron x-ray micro-computed tomography (XCT) at the European Synchrotron Radiation Facility. This replicator was designed to extend the characterization of L-PBF to 3D. This instrument fills in a technical gap because the existing replicators were mostly designed to shed light on the dynamic mechanisms involved in molten pool formation but, therefore, suffered from a lack of 3D information. Technical details regarding the setup and beamline integration are given. Experimental validations via post-mortem XCT scans and in situ scans acquired during experiments conducted at the BM05 beamline of the European Synchrotron Radiation Facility are provided. Based on a few illustrative examples, we show that such a replicator opens the path to collect key 3D information that to date could not be available. Our miniature instrument complements the other replicators developed in the world by other research groups that enable operando x-ray imaging (radiography) and operando x-ray diffraction.

Reconstructing dual-phase nanometer scale grains within a pearlitic steel tip in 3D through 4D-scanning precession electron diffraction tomography and automated crystal orientation mapping.

The properties of polycrystalline materials are related to their microstructures and hence a complete description, including size, shape, and orientation of the grains, is necessary to understand the behavior of materials. Here, we use Scanning Precession Electron Diffraction (SPED) in the Transmission Electron Microscope (TEM) combined with a tilt series to reconstruct individual grains in 3D within a polycrystalline dual-phase cold wire-drawn pearlitic steel sample. Nanoscale ferrite grains and intragranular cementite particles were indexed using an Automated Crystallographic Orientation Mapping (ACOM) tool for each tilt dataset. The grain orientations were tracked through the tilt datasets and projections of the individual grains were reconstructed from the diffraction data using an orientation-specific Virtual Dark Field (VDF) approach for tomographic reconstruction. The algorithms used to process and reconstruct such datasets are presented. These algorithms represent an extension to the ACOM approach that may be straightforwardly applied to other multi-phase polycrystalline materials to enable 3D spatial and orientation reconstructions.

High-temperature deformation followed in situ by X-ray microtomography: a methodology to track features under large strain.

Metallic materials processing such as rolling, extrusion or forging often involves high-temperature deformation. Usually under such conditions the samples are characterized post mortem, under pseudo in situ conditions with interrupted tests, or in situ with a limited strain rate. A full in situ 3D characterization, directly during high-temperature deformation with a prescribed strain-rate scheme, requires a dedicated sample environment and a dedicated image-analysis workflow. A specific sample environment has been developed to enable highly controlled (temperature and strain rate) high-temperature deformation mechanical testing to be conducted while performing in situ tomography on a synchrotron beamline. A dedicated digital volume correlation algorithm is used to estimate the strain field and track pores while the material endures large deformations. The algorithm is particularly suitable for materials with few internal features when the deformation steps between two images are large. An example of an application is provided: a high-temperature compression test on a porous aluminium alloy with individual pore tracking with a specific strain-rate scheme representative of rolling conditions.

Arthropod entombment in weathering-formed opal: new horizons for recording life in rocks.

Animal fossils preserved in various geological materials, such as limestone, claystone, or amber, provide detailed information on extinct species that is indispensable for retracing the evolution of terrestrial life. Here, we present the first record of an animal fossil preserved in opal formed by weathering with such high-resolution details that even individual cuticle hairs are observed. The fossil consists of the exoskeleton of a nymphal insect belonging to the order Hemiptera and either the family Tettigarctidae or the Cicadidae. This identification is based on anatomical details such as the tibial and femoral morphology of the forelegs. The exoskeleton of the insect was primarily zeolitized during the alteration of the host rocks and later sealed in opal deposited by silica-rich fluids derived from the continental weathering of the volcanic host rocks. Organic matter is preserved in the form of amorphous carbon. This finding makes opal formed by rocks weathering a new, complementary source of animal fossils, offering new prospects for the search for ancient life in the early history of Earth and possibly other terrestrial planets such as Mars, where weathering-formed opal occurs.

Solvent-free preparation of porous poly(l-lactide) microcarriers for cell culture.

Porous polymeric microcarriers are a versatile class of biomaterial constructs with extensive use in drug delivery, cell culture and tissue engineering. Currently, most methods for their production require potentially toxic organic solvents with complex setups which limit their suitability for biomedical applications and their large-scale production. Herein, we report an organic, solvent-free method for the fabrication of porous poly(l-lactide) (PLLA) microcarriers. The method is based on the spherulitic crystallization of PLLA in its miscible blends with poly(ethylene glycol) (PEG). It is shown that the PLLA spherulites are easily recovered as microcarriers from the blends by a water-based process. Independent control over microcarrier size and porosity is demonstrated, with a higher crystallization temperature leading to a larger size, and a higher PLLA content in the starting blend resulting in a lower microcarrier porosity. Microcarriers are shown to be biocompatible for the culture of murine myoblasts and human adipose stromal/stem cells (hASC). Moreover, they support not only the long-term proliferation of both cell types but also hASC differentiation toward osseous tissues. Furthermore, while no significant differences are observed during cell proliferation on microcarriers of two different porosities, microcarriers of lower porosity induce a stronger hASC osteogenic differentiation, as evidenced by higher ALP enzymatic activity and matrix mineralization. Consequently, the proposed organic-solvent-free method for the fabrication of biocompatible porous PLLA microcarriers represents an innovative methodology for ex vivo cell expansion and its application in stem cell therapy and tissue engineering. STATEMENT OF SIGNIFICANCE: We report a new solvent-free method for the preparation of porous polymeric microcarriers for cell culture, based on biocompatible poly(l-lactide), with independently controllable size and porosity. This approach, based on the spherulitic crystallization in polymer blends, offers the advantages of simple implementation, biological and environmental safety, easy adaptability and up-scalablility. The suitability of these microcarriers is demonstrated for long-term culture of both murine myoblasts and human adipose stromal/stem cells (hASCs). We show that prepared microcarriers support the osteogenic differentiation of hASCs, provided microcarriers of properly-tuned porosity are used. Hence, this new method is an important addition to the arsenal of microcarrier fabrication techniques, which will contribute to the adoption, regulatory approval and eventually clinical availability of microcarrier-based treatments and therapies.

MHz frame rate hard X-ray phase-contrast imaging using synchrotron radiation.

Third generation synchrotron light sources offer high photon flux, partial spatial coherence, and ~10-10 s pulse widths. These enable hard X-ray phase-contrast imaging (XPCI) with single-bunch temporal resolutions. In this work, we exploited the MHz repetition rates of synchrotron X-ray pulses combined with indirect X-ray detection to demonstrate the potential of XPCI with millions of frames per second multiple-frame recording. This allows for the visualization of aperiodic or stochastic transient processes which are impossible to be realized using single-shot or stroboscopic XPCI. We present observations of various phenomena, such as crack tip propagation in glass, shock wave propagation in water and explosion during electric arc ignition, which evolve in the order of km/s (µm/ns).