Hydride formation and dynamic phase changes during template-assisted Pd electrodeposition.

We investigated the structural evolution of electrochemically fabricated Pd nanowiresin situby means of grazing-incidence transmission small- and wide-angle x-ray scattering (GTSAXS and GTWAXS), x-ray fluorescence (XRF) and two-dimensional surface optical reflectance (2D-SOR). This shows how electrodeposition and the hydrogen evolution reaction (HER) compete and interact during Pd electrodepositon. During the bottom-up growth of the nanowires, we show thatß-phase Pd hydride is formed. Suspending the electrodeposition then leads to a phase transition fromß-phase Pd hydride toα-phase Pd. Additionally, we find that grain coalescence later hinders the incorporation of hydrogen in the Pd unit cell. GTSAXS and 2D-SOR provide complementary information on the volume fraction of the pores occupied by Pd, while XRF was used to monitor the amount of Pd electrodeposited.

Evaluating the Suitability of 3D Bioprinted Samples for Experimental Radiotherapy: A Pilot Study.

Radiotherapy is an important component in the treatment of lung cancer, one of the most common cancers worldwide, frequently resulting in death within only a few years of diagnosis. In order to evaluate new therapeutic approaches and compare their efficiency with regard to tumour control at a pre-clinical stage, it is important to develop standardized samples which can serve as inter-institutional outcome controls, independent of differences in local technical parameters or specific techniques. Recent developments in 3D bioprinting techniques could provide a sophisticated solution to this challenge. We have conducted a pilot project to evaluate the suitability of standardized samples generated from 3D printed human lung cancer cells in radiotherapy studies. The samples were irradiated at high dose rates using both broad beam and microbeam techniques. We found the 3D printed constructs to be sufficiently mechanically stable for use in microbeam studies with peak doses up to 400 Gy to test for cytotoxicity, DNA damage, and cancer cell death in vitro. The results of this study show how 3D structures generated from human lung cancer cells in an additive printing process can be used to study the effects of radiotherapy in a standardized manner.

Swelling of Ti3 C2 Tx MXene in Water and Methanol at Extreme Pressure Conditions.

Pressure-induced swelling has been reported earlier for several hydrophilic layered materials. MXene Ti3C2Tx is also a hydrophilic layered material composed by 2D sheets but so far pressure-induced swelling is reported for this material only under conditions of shear stress at MPa pressures. Here, high-pressure experiments are performed with MXenes prepared by two methods known to provide "clay-like" materials. MXene synthesized by etching MAX phase with HCl+LiF demonstrates the effect of pressure-induced swelling at 0.2 GPa with the insertion of additional water layer. The transition is incomplete with two swollen phases (ambient with d(001) = 16.7Å and pressure-induced with d(001) = 19.2Å at 0.2 GPa) co-existing up to the pressure point of water solidification. Therefore, the swelling transition corresponds to change from two-layer water intercalation (2L-phase) to a never previously observed three-layer water intercalation (3L-phase) of MXene. Experiments with MXene prepared by LiCl+HF etching have not revealed pressure-induced swelling in liquid water. Both MXenes also show no anomalous compressibility in liquid methanol. The presence of pressure-induced swelling only in one of the MXenes indicates that the HCl+LiF synthesis method is likely to result in higher abundance of hydrophilic functional groups terminating 2D titanium carbide.

HAT: a high-energy surface X-ray diffraction analysis toolkit.

This work introduces the high-energy surface X-ray diffraction analysis toolkit (HAT), an open-source cross-platform software package written in Python to allow the extraction and processing of high-energy surface X-ray diffraction (HESXRD) data sets. Thousands of large-area detector images are collected in a single HESXRD scan, corresponding to billions of pixels and hence reciprocal space positions. HAT is an optimized reciprocal space binner that implements a graphical user interface to allow the easy and interactive exploration of HESXRD data sets. Regions of reciprocal space can be selected with movable and resizable masks in multiple views and are projected onto different axes to allow the creation of reciprocal space maps and the extraction of crystal truncation rods. Current and future versions of HAT can be downloaded and used free of charge.

The Oxygen Evolution Reaction Drives Passivity Breakdown for Ni-Cr-Mo Alloys.

Corrosion is the main factor limiting the lifetime of metallic materials, and a fundamental understanding of the governing mechanism and surface processes is difficult to achieve since the thin oxide films at the metal-liquid interface governing passivity are notoriously challenging to study. In this work, a combination of synchrotron-based techniques and electrochemical methods is used to investigate the passive film breakdown of a Ni-Cr-Mo alloy, which is used in many industrial applications. This alloy is found to be active toward oxygen evolution reaction (OER), and the OER onset coincides with the loss of passivity and severe metal dissolution. The OER mechanism involves the oxidation of Mo4+ sites in the oxide film to Mo6+ that can be dissolved, which results in passivity breakdown. This is fundamentally different from typical transpassive breakdown of Cr-containing alloys where Cr6+ is postulated to be dissolved at high anodic potentials, which is not observed here. At high current densities, OER also leads to acidification of the solution near the surface, further triggering metal dissolution. The OER plays an important role in the mechanism of passivity breakdown of Ni-Cr-Mo alloys due to their catalytic activity, and this effect needs to be considered when studying the corrosion of catalytically active alloys.

MiniMelt: An instrument for real-time tracking of electron beam additive manufacturing using synchrotron x-ray techniques.

The development of a sample environment for in situ x-ray characterization during metal Electron Beam Powder Bed Fusion (PBF-EB), called MiniMelt, is presented. The design considerations, the features of the equipment, and its implementation at the synchrotron facility PETRA III at Deutsches Elektronen-Synchrotron, Hamburg, Germany, are described. The equipment is based on the commercially available Freemelt ONE PBF-EB system but has been customized with a unique process chamber to enable real-time synchrotron measurements during the additive manufacturing process. Furthermore, a new unconfined powder bed design to replicate the conditions of the full-scale PBF-EB process is introduced. The first radiography (15 kHz) and diffraction (1 kHz) measurements of PBF-EB with a hot-work tool steel and a Ni-base superalloy, as well as bulk metal melting with the CMSX-4 alloy, using the sample environment are presented. MiniMelt enables time-resolved investigations of the dynamic phenomena taking place during multi-layer PBF-EB, facilitating process understanding and development of advanced process strategies and materials for PBF-EB.

Microstructural Constituents and Mechanical Properties of Low-Density Fe-Cr-Ni-Mn-Al-C Stainless Steels.

Metallic material concepts associated with the sustainable and efficient use of resources are currently the subject of intensive research. Al addition to steel offers advantages in view of lightweight, durability, and efficient use of high-Fe scrap from the Al industry. In the present work, Al was added to Fe-12Cr-(9,12)Ni-3Mn-0.3C-xAl (x = 0.1-6) (wt.%) stainless steels to assess its influence on microstructure and mechanical properties. According to density measurements based on Archimedes' principle, densities were between 7.70 and 7.08 g/cm3. High-energy X-ray diffraction estimations of the lattice parameter indicated that nearly 31% of density reduction was caused by the lattice expansion associated with Al addition. Depending on Al concentration, austenitic and duplex matrix microstructures were obtained at room temperature. In the presence of up to 3 wt.% Al, the microstructure remained austenitic. At the same time, strength and hardness were slightly enhanced. Al addition in higher quantities resulted in the formation of duplex matrix microstructures with enhanced yield strength but reduced ductility compared to the austenitic alloys. Due to the ready formation of B2-(Ni,Fe)Al intermetallics in the ferrite phase of the present alloy system, the increase in strength due to the presence of ferrite was more pronounced compared to standard duplex stainless steels. The occurrence of B2 intermetallics was implied by dilatometry measurements and confirmed by electron microscopy examinations and high-energy X-ray diffraction measurements.

Powder diffraction computed tomography: a combined synchrotron and neutron study.

Diffraction and imaging using x-rays and neutrons are widely utilized in different fields of engineering, biology, chemistry and/or materials science. The additional information gained from the diffraction signal by x-ray diffraction and computed tomography (XRD-CT) can give this method a distinct advantage in materials science applications compared to classical tomography. Its active development over the last decade revealed structural details in a non-destructive way with unprecedented sensitivity. In the current contribution an attempt to adopt the well-established XRD-CT technique for neutron diffraction computed tomography (ND-CT) is reported. A specially designed 'phantom', an object displaying adaptable contrast sufficient for both XRD-CT and ND-CT, was used for method validation. The feasibility of ND-CT is demonstrated, and it is also shown that the ND-CT technique is capable to provide a non-destructive view into the interior of the 'phantom' delivering structural information consistent with a reference XRD-CT experiment.

A rotational and axial motion system load frame insert for in situ high energy x-ray studies.

High energy x-ray characterization methods hold great potential for gaining insight into the behavior of materials and providing comparison datasets for the validation and development of mesoscale modeling tools. A suite of techniques have been developed by the x-ray community for characterizing the 3D structure and micromechanical state of polycrystalline materials; however, combining these techniques with in situ mechanical testing under well characterized and controlled boundary conditions has been challenging due to experimental design requirements, which demand new high-precision hardware as well as access to high-energy x-ray beamlines. We describe the design and performance of a load frame insert with a rotational and axial motion system that has been developed to meet these requirements. An example dataset from a deforming titanium alloy demonstrates the new capability.

Strain-dependent deformation behavior in nanocrystalline metals.

The deformation behavior as a function of applied strain was studied in a nanostructured Ni-Fe alloy using the in situ synchrotron diffraction technique. It was found that the plastic deformation process consists of two stages, undergoing a transition with applied strain. At low strains, the deformation is mainly accommodated at grain boundaries, while at large strains, the dislocation motion becomes probable and eventually dominates. In addition, current results revealed that, at small grain sizes, the 0.2% offset criterion cannot be used to define the macroscopic yield strength any more. The present study also explained the controversial observations in the literature.

Synchrotron applications of an amorphous silicon flat-panel detector.

A GE Revolution 41RT flat-panel detector (GE 41RT) from GE Healthcare (GE) has been in operation at the Advanced Photon Source for over two years. The detector has an active area of 41 cm x 41 cm with 200 microm x 200 microm pixel size. The nominal working photon energy is around 80 keV. The physical set-up and utility software of the detector system are discussed in this article. The linearity of the detector response was measured at 80.7 keV. The memory effect of the detector element, called lag, was also measured at different exposure times and gain settings. The modulation transfer function was measured in terms of the line-spread function using a 25 microm x 1 cm tungsten slit. The background (dark) signal, the signal that the detector will carry without exposure to X-rays, was measured at three different gain settings and with exposure times of 1 ms to 15 s. The radial geometric flatness of the sensor panel was measured using the diffraction pattern from a CeO(2) powder standard. The large active area and fast data-capturing rate, i.e. 8 frames s(-1) in radiography mode, 30 frames s(-1) in fluoroscopy mode, make the GE 41RT one of a kind and very versatile in synchrotron diffraction. The loading behavior of a Cu/Nb multilayer material is used to demonstrate the use of the detector in a strain-stress experiment. Data from the measurement of various samples, amorphous SiO(2) in particular, are presented to show the detector effectiveness in pair distribution function measurements.

Formation and subdivision of deformation structures during plastic deformation.

During plastic deformation of metals and alloys, dislocations arrange in ordered patterns. How and when these self-organization processes take place have remained elusive, because in situ observations have not been feasible. We present an x-ray diffraction method that provided data on the dynamics of individual, deeply embedded dislocation structures. During tensile deformation of pure copper, dislocation-free regions were identified. They showed an unexpected intermittent dynamics, for example, appearing and disappearing with proceeding deformation and even displaying transient splitting behavior. Insight into these processes is relevant for an understanding of the strength and work-hardening of deformed materials.