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All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

A practical guide for crystal growth of van der Waals layered materials

This Tutorial provides an overview of the techniques that are most commonly utilized to grow bulk van der Waals crystals. The materials discussed were selected to highlight various challenges that are often encountered during crystal growth. Additionally, in relatively equal parts, the text covers melt-based techniques, vapor transport growths, and the characterization of crystal quality with an emphasis on structural and chemical homogeneities. Furthermore, pertinent details are given regarding the growth and characterization of many specific compounds, with examples mostly drawn from our own research, and an effort is made to highlight cases where the growths offer a particular lesson or the conditions have a significant impact on the crystal’s physical properties. A primary goal is to motivate more researchers to grow crystals by providing general descriptions and considerations for different growth techniques and equipment while sharing some of our own lessons learned and best practices for the growth and characterization of layered van der Waals crystals. The Tutorial is not written solely for aspiring crystal growers, however, because any researcher who collaborates with a crystal grower can benefit from having a greater understanding and appreciation of the processes of crystal growth and materials development.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Graphene nanopattern as a universal epitaxy platform for single-crystal membrane production and defect reduction

Heterogeneous integration of single-crystal materials offers great opportunities for advanced device platforms and functional systems. Although substantial efforts have been made to co-integrate active device layers by heteroepitaxy, the mismatch in lattice polarity and lattice constants has been limiting the quality of the grown materials. Layer transfer methods as an alternative approach, on the other hand, suffer from the limited availability of transferrable materials and transfer-process-related obstacles. Here, we introduce graphene nanopatterns as an advanced heterointegration platform that allows the creation of a broad spectrum of freestanding single-crystalline membranes with substantially reduced defects, ranging from non-polar materials to polar materials and from low-bandgap to high-bandgap semiconductors. Additionally, we unveil unique mechanisms to substantially reduce crystallographic defects such as misfit dislocations, threading dislocations and antiphase boundaries in lattice- and polarity-mismatched heteroepitaxial systems, owing to the flexibility and chemical inertness of graphene nanopatterns. More importantly, we develop a comprehensive mechanics theory to precisely guide cracks through the graphene layer, and demonstrate the successful exfoliation of any epitaxial overlayers grown on the graphene nanopatterns. Furthermore, this approach has the potential to revolutionize the heterogeneous integration of dissimilar materials by widening the choice of materials and offering flexibility in designing heterointegrated systems.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2024

In situ counter-diffusion crystallization and long-term crystal preservation in microfluidic fixed targets for serial crystallography

Compared with batch and vapor diffusion methods, counter diffusion can generate larger and higher-quality protein crystals yielding improved diffraction data and higher-resolution structures. Typically, counter-diffusion experiments are conducted in elongated chambers, such as glass capillaries, and the crystals are either directly measured in the capillary or extracted and mounted at the X-ray beamline. Despite the advantages of counter-diffusion protein crystallization, there are few fixed-target devices that utilize counter diffusion for crystallization. In this article, different designs of user-friendly counter-diffusion chambers are presented which can be used to grow large protein crystals in a 2D polymer microfluidic fixed-target chip. Methods for rapid chip fabrication using commercially available thin-film materials such as Mylar, propylene and Kapton are also detailed. Rules of thumb are provided to tune the nucleation and crystal growth to meet users' needs while minimizing sample consumption. These designs provide a reliable approach to forming large crystals and maintaining their hydration for weeks and even months. This allows ample time to grow, select and preserve the best crystal batches before X-ray beam time. Importantly, the fixed-target microfluidic chip has a low background scatter and can be directly used at beamlines without any crystal handling, enabling crystal quality to be preserved. The approach is demonstrated with serial diffraction of photoactive yellow protein, yielding 1.32 Å resolution at room temperature. Fabrication of this standard microfluidic chip with commercially available thin films greatly simplifies fabrication and provides enhanced stability under vacuum. These advances will further broaden microfluidic fixed-target utilization by crystallographers.

Liu, Zhongrui↗
DOE OSTI2021

Computationally Guided Discovery of Axis-Dependent Conduction Polarity in NaSnAs Crystals

Most electronic materials exhibit a single dominant charge carrier type, either holes or electrons, along all crystallographic directions. However, there are a small number of compounds, mostly metals, that exhibit simultaneous p-type and n-type conduction behavior along different crystallographic directions. We demonstrate that the experimental discovery of semiconductors with this axis-dependent conduction polarity can be facilitated by identifying a large anisotropy of either the electron or hole effective masses (m*) or both, providing the electron and hole masses dominate along different crystallographic directions. We calculated the layered semiconductor NaSnAs to have a lower electron m* in-plane than the cross-plane and a very large hole m* in-plane and small hole m* cross-plane. We established the growth of >3 mm-sized NaSnAs crystals via Sn flux and confirmed the band gap to be 0.65 eV, in agreement with theory. NaSnAs exhibits p-type thermopowers cross-plane and n-type thermopowers in-plane, confirming that the large anisotropy in the effective mass at the band edges is an excellent indicator for axis-dependent conduction polarity. Altogether, this work shows that the discovery of semiconductors with such a phenomenon can be accelerated by computationally evaluating the anisotropic curvatures of the band edges, paving the way for their future discovery and application.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2024

Prediction of microstructure formation in laser powder bed fusion process.

The datasets are results analyzing the predicted microstructures in a single track during the laser powder bed fusion additive manufacturing process. They are the outputs by running the opensource code, muMatScale (The code can be cited at: Yuan, Lang, Fattebert, Jean-Luc, and Sabau, Adrian. (2023, August 03). muMatScale. [Computer software]. https://github.com/lang-yuan/muMatScale. https://doi.org/10.11578/dc.20240112.2.) For each set of data, it contains the time-dependent information of Temperature, Fraction Solid, Grain ID, Grain Angle ( crystallographic orientations by Euler angles), and solute Composition. The dataset can be visualized by Paraview (https://www.paraview.org/ ). The 6 datasets are: 1. Baseline_base1_n4e14_dt20: baseline case with bulk nucleation density of 4E+14/m^3, undercooling of 20K, substrate nucleation density of 1.5E+15/m^3 2. Nuc_n4e15_dt20: case with bulk nucleation density of 4E+15/m^3, undercooling of 20K, substrate nucleation density of 1.5E+15/m^3 3. Nuc_n4e15_dt50: case with bulk nucleation density of 4E+15/m^3, undercooling of 50K, substrate nucleation density of 1.5E+15/m^3 4. Nuc_n6e15_dt20: case with bulk nucleation density of 4E+16/m^3, undercooling of 20K, substrate nucleation density of 1.5E+15/m^3 5. Base4_n4e14_dt20: case with bulk nucleation density of 4E+14/m^3, undercooling of 20K, substrate nucleation density of 6.0E+15/m^3 6. Base16_n4e14_dt20: case with bulk nucleation density of 4E+14/m^3, undercooling of 20K, substrate nucleation density of 2.4E+16/m^3

36 MATERIALS SCIENCE↗
DOE OSTI2021

Anhydrous vs Hydrated f-Element Acetate Polymers Dictated by the Stoichiometry of Protic Acidic/Basic Azole Mixtures

Continuing our investigations of ionic liquid (IL) based routes to a library of f-element/soft donor complexes which could be studied crystallographically, we have explored the dissolution of f-element salts in protic imidazole-based ILs containing only soft donors at high temperatures to drive off volatiles, including water and carboxylic or mineral acids. Here we present our results, reacting acidic and basic azoles in 1:3 or 1:1 stoichiometric compositions at elevated temperature, followed by saturation with Nd(OAc) 3 ·xH 2 O or Ce(OAc) 3 ·xH 2 O, which led to 13 new metal–acetate polymeric complexes identified by single-crystal X-ray diffraction. We found that the diversity in coordination modes of the simple acetate ligand that interfere with substitution of the softer N donors led to several readily crystallizable complexes forming two distinct groups with respect to f-element interaction with the ionic liquid precursors. When the acidic/basic azole ratio was 1:3, acetate and a neutral basic azole were found to be coordinated to the metal centers but no water, although in one case (2) water was observed in the secondary coordination sphere: [Ce(μ 2 -OAc) 3 (C 1 im)] n (1, C 1 im = 1-methylimidazole), [Nd(μ 2 -(OAc) 3 (C 1 im)] n ·nH 2 O (2), [Ce(μ 2 -OAc) 3 (C 2 im)] n (3, C 2 im = 1-ethylimidazole), [Ln(μ 2 -OAc) 3 DMF] n (Ln = Nd (4), Ce (5); dimethylformamide (DMF) was substituted for the azole mixture), and [Nd(μ 2 -OAc) 3 (C 4 im)] n (6, C 4 im = 1-butylimidazole). However, when the stoichiometric ratio was 1:1, water was always observed coordinated to the metal ions with the acidic azole included in the structure as a solvate or cocrystal, despite a higher reaction temperature: [Nd(μ 2 -OAc) 3 (OH 2 )] n ·n(1,2,3-Taz) (7, 1,2,3-Taz = 1,2,3-triazole), [Ln(μ 2 -OAc) 3 (OH 2 )] n ·n(4,5-DCim) (Ln = Nd (8), Ce (9), 4,5-DCim = 4,5-dicyanoimidazole), [Ln(μ 2 -OAc) 3 (OH 2 )] n ·n(3,5-diNH 2 -1,2,4-Taz) (Ln = Nd (10), Ce (11), 3,5-diNH 2 -1,2,4-Taz = 3,5-diamino-1,2,4-triazole), [Ce(μ 2 -OAc) 3 (OH 2 )] n ·n(3-NH 2 -1,2,4-Taz) (12, 3-NH 2 -1,2,4-Taz = 3-amino-1,2,4-triazole), and [Nd(μ 2 -OAc) 3 (OH 2 )] n ·n(5-NH 2 -Tz) (13, 5-NH2-Tz = 5-aminotetrazole). All of the compounds retain the Ln:OAc– ratio of 1:3 and form 1D polymeric chains; however, they exhibit a variety of coordination modes affecting the degree of chain condensation. The isolation of both hydrated and anhydrous products revealed different abilities of the investigated soft N-donors to compete with O-donors finding their place in the coordination sphere of the lanthanide or in the crystal lattice.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Breaking atomic-level ordering via biaxial strain in functional oxides: A DFT study

Oxygen vacancies are found to play a crucial role in inducing many functional properties at the heterointerfaces in complex oxides. Gaining better control over the properties requires an understanding of the atomic structure of oxygen vacancies at the heterointerfaces. In this paper, we elucidate the effects of the interfacial strain on the oxygen-vacancy ordering in fluorite δ-Bi 2 O 3 and perovskite LaNiO 2.5 using first-principles calculations. By applying biaxial strains, we find that the <110>-<111> oxygen vacancy order in δ-Bi2O3 is broken, resulting in a faster diffusion of oxygen ions. Similarly, the biaxial strain is used to leverage both ordered and disordered arrangements of vacancies in LaNiO 2.5 . Besides the vacancy order, we find that the biaxial strain can also be used to break the cation order in Gd 2 Ti 2 O 7 , where Gd and Ti antisites can be created on the cation sublattice, which leads to enhanced radiation tolerance and higher oxygen diffusivity. Overall, these results indicate that the biaxial strain that is commonly present at heterointerfaces can be used to gain control over both ordered and disordered arrangements of defects, potentially opening new opportunities to functionalize complex oxides.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Structure of V-defects in long wavelength GaN-based light emitting diodes

The V-defect is a naturally occurring inverted hexagonal pyramid structure that has been studied in GaN and InGaN growth since the 1990s. Strategic use of V-defects in pre-quantum well superlattices or equivalent preparation layers has enabled record breaking efficiencies for green, yellow, and red InGaN light emitting diodes (LEDs) utilizing lateral injection of holes through the semi-polar sidewalls of the V-defects. In this article, we use advanced characterization techniques such as scattering contrast transmission electron microscopy, high angle annular dark field scanning transmission electron microscopy, x-ray fluorescence maps, and atom probe tomography to study the active region compositions, V-defect formation, and V-defect structure in green and red LEDs grown on (0001) patterned sapphire and (111) Si substrates. We identify two distinct types of V-defects. The “large” V-defects are those that form in the pre-well superlattice and promote hole injection, usually nucleating on mixed (Burgers vector b = ±a±c⁠) character threading dislocations. In addition, “small” V-defects often form in the multi-quantum well region and are believed to be deleterious to high-efficiency LEDs by providing non-radiative pathways. The small V-defects are often associated with basal plane stacking faults or stacking fault boxes. Furthermore, we show through scattering contrast transmission electron microscopy that during V-defect filling, the threading dislocation, which runs up the center of the V-defect, will “bend” onto one of the six {10$\overline{1}$1} semi-polar planes. In conclusion, this result is essential to understanding non-radiative recombination in V-defect engineered LEDs.

42 ENGINEERING↗
DOE OSTI2025

Combined molecular and spin dynamics simulation of BCC iron with vacancy defects

Utilizing an atomistic computational model, which handles both translational and spin degrees of freedom, combined molecular and spin dynamics simulations have been performed to investigate the effect of vacancy defects on spin wave excitations in ferromagnetic iron. Fourier transforms of space- and time-displaced correlation functions yield the dynamic structure factor, providing characteristic frequencies and lifetimes of the spin wave modes. A comparison of the system with a 5% vacancy concentration with pure lattice data shows a decrease in frequency and a decrease in lifetime for all transverse spin wave excitations observed. In addition, the clearly defined transverse spin wave excitations are distorted with the introduction of vacancy defects, and we observe reduced excitation lifetimes due to increased magnon–magnon scattering. We observe further evidence of increased magnon–magnon scattering, as the peaks in the longitudinal spin wave spectrum become less distinct. Finally, similar impacts are observed in the vibrational subsystem, with a decrease in characteristic phonon frequency and flattening of lattice excitation signals due to vacancy defects.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Electron beam irradiation effects on bulk metals: a comparative study of polycrystalline versus single-crystalline structures

This study investigates the effects of electron beam (e-beam) irradiation on the mechanical and structural properties of eight bulk metallic samples, comprising both polycrystalline (PC) and single-crystalline (SC) forms of Ni, Cr, V, and Ti. These metals were evaluated as potential candidates for beam exit windows in high-power (MW-class) particle accelerators. The primary objective is to identify metals capable of withstanding the conditions of high-power/MW-class e-beam accelerators and serve effectively as exit windows. Selection criteria were based on each metal’s intrinsic properties, power dissipation capability, and irradiation-induced changes in mechanical behavior, including hardness, elastic modulus, and defect density. Comprehensive characterization was conducted using field-emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM–EDS), X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and nanoindentation, performed both before and after exposure to a ~¿66 kGy dose from a 10 MeV e-beam accelerator. Results revealed that e-beam irradiation induced hardening in PC Ni, whereas PC Ti, commonly used in beam exit windows, exhibited softening. The observed softening in PC Ti is attributed to grain coarsening, elongation, and the formation of twins and twin boundaries, in contrast to the smaller, compressed grains in the pristine (Pr) PC Ti samples, consistent with the Hall–Petch relationship. The stresses due to twinning are small and insignificant in influencing the overall hardening of the PC Ti irradiated sample when compared to the stresses due to the dislocation density. Conversely, SC Ti samples exhibited irradiation-induced hardening. The SC Ti irradiated samples developed additional irradiation-induced modifications in crystallographic texture of (100), (101), (110), (200), (112), (004), and (211) as evidenced from the XRD results, which could probably explain the hardening effect that is caused by irradiation.

36 MATERIALS SCIENCE↗
NASA NTRS1998

New AFM Techniques for Investigating Molecular Growth Mechanisms of Protein Crystals

Atomic Force Microscopy (AFM) has emerged as a powerful technique for investigating protein crystal growth. Earlier AFM studies were among the first to demonstrate that these crystals grew by dislocation and 2D nucleation growth mechanisms [1]. These investigations were restricted to the micron range where only surface features, such as dislocation hillocks and 2D islands are visible. Most AFM instruments can scan at higher resolutions and have the potential to resolve individual protein molecules at nanometer ranges. Such scans are essential for determining the molecular packing arrangements on crystal faces and for probing the growth process at the molecular level. However, at this resolution the AFM tip influences the image produced, with the resulting image being a convolution of the tip shape and the surface morphology [2]. In most studies this problem is resolved by deconvoluting the image to obtain the true surface morphology. Although deconvolution routines work reasonably well for simple one- dimensional shapes, for complex surfaces this approach does not produce accurate results. In this study we devised a new approach which takes advantage of the precise molecular order of crystal surfaces, combined with the knowledge of individual molecular shapes from the crystallographic data of the protein and the AFM tip shape. This information is used to construct expected theoretical AFM images by convoluting the tip shape with the constructed crystal surface shape for a given surface packing arrangement. By comparing the images from actual AFM scans with the constructed ones for different possible surface packing arrangements, the correct packing arrangement can be conclusively determined. This approach was used in this study to determine the correct one from two possible packing arrangements on (I 10) faces of tetragonal lysozyme crystals. Another novel AFM technique was also devised to measure the dimension of individual growth units of the crystal faces. Measuring these units was not attempted before and most studies have assumed that the growth unit consisted of individual protein molecules. The linescan mode of AFM instruments allows the crystal surface to be scanned along a single line. By scanning across a growth step an image showing the motion of the step is obtained. Normally such an image shows a straight line for continuous and constant step velocity. In this study by increasing the scan rate and by decreasing the step velocity (by decreasing the supersaturation), we were able to capture images of individual growth events, shown by jump discontinuities in the step line. By suitable integration of the image the growth unit dimension in the scanned direction can be obtained. Since multiple units can be involved in the growth process it is necessary to collect a statistically relevant sample before drawing conclusions about the growth mechanism. This technique was successfully employed to obtain the dimensions of growth units for the (110) face, showing that they consisted of various aggregates corresponding to the 43 helices in the crystal structure.

Li, Huayu↗
DOE OSTI2025

Review of radiation-induced defects in GaAs

Radiation-resilient optoelectronic materials are highly desired in space and nuclear applications, and understanding the relevant defects and electronic processes in those materials is crucial for both current and next-generation applications. GaAs is a prototypical semiconductor that serves as a foundational system for describing and understanding optoelectronic devices. In this review, both experimental studies and molecular dynamics (MD) simulations of irradiated GaAs are reviewed, with particular emphasis on the deep-level transient spectroscopy, irradiation-induced amorphization zones, and MD predictions of damage structures. The MD results are also compared to predictions of the non-ionized energy-loss model. Recent theoretical studies, in particular, density functional theory based calculations on the simple intrinsic defects and defect clusters in GaAs, are also reviewed. These defects have an important role in dictating the evolution of GaAs in radiation damage environments, as they impact the coupled dynamics of charge carriers. Finally, possible gaps and challenges toward the general understanding of defect evolution in GaAs are discussed.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Deciphering Extreme Mineral Records; Microstructural Phase Heritage of Shocked Materials

High-pressure minerals such as coesite, stishovite, and reidite are often used as indicators of shock metamorphism. However, high-pressure and high-temperature phases are metastable at ambient conditions and, therefore, often revert to a more energetically favorable phase. During solid-state transformations, the crystallographic orientations of the stable polymorph are controlled by the transformation pathway from the parent. Microstructural orientation analysis using electron backscatter diffraction (EBSD) of the stable phase can reveal systematic intercrystalline orientation relationships (OR) diagnostic of solid-state transformations from these high-pressure or high-temperature polymorph phases (Cayron et al., 2006). Knowledge of polymorph stability fields for a given system can thus be used to infer minimum shock P and/or T conditions that rocks have experienced, which are otherwise unavailable using traditional thermobarometers such as element partition coefficients. Using orientation relationships to infer the former presence of mineral phases has been termed microstructural “phase heritage”, and has successfully been used to probe for evidence of extreme pressures and temperatures resulting from hypervelocity impacts. The reconstruction of polymorphs of ZrSiO4 (zircon, reidite) and ZrO2 (baddeleyite) have further elucidated the behavior of these phases under hypervelocity impact conditions (Timms et al., 2017a; White et al., 2018), and OR analysis of shocked monazite has identified a previously unrecognized tetragonal high-P polymorph (Erickson et al., 2019). Zircon will convert to the low tetragonal polymorph reidite at shock stresses above ~21 GPa. However, upon decompression at temperatures above 1200 °C reidite will revert to zircon (Kusaba et al., 1985). Recrystallized zircon neoblasts encased in impact melt often show systematic misorientation relationships of 90° about <110> indicative of reversion from the reidite (Fig. 1), and preserving cryptic evidence of the high-P history that is often erased by the post shock thermal spike (Cavosie et al., 2016). Microstructural OR analysis of a dissociated zircon corona composed of baddeleyite (monoclinic-ZrO2) has identified the former presence of cubic zirconia within impact melt glass from the Mistastin Lake impact structure, Labrador, CA. Based on stability fields in the ZrO2-SiO2 binary phase diagram, cubic zirconia records thermal conditions in excess of 2370 °C at ambient P, indicating that the Mistastin impact melt is the hottest rock identified on Earth’s surface (Timms et al., 2017b). Shock-deformed monazite (monoclinic La,Ce,ThPO4) containing lamellae comprised of interlocking laths has been identified from the Haughton Dome impact structure, Nunavut, Canada and Nördlinger-Ries Crater, southern Germany. The lath-structured lamellae are composed of four systematic orientation variants, which OR analyses indicate originate from a tetragonal parent whereby the [010]monoclinic aligns with either [100] or [010]tetragonal (Erickson et al., 2019). These results highlight utility of microstructural phase heritage analyses for the identification of unstable high-P or high-T polymorphs that uniquely record the extremely transient shock conditions produced by hypervelocity impacts.

Timmons Erickson↗
DOE OSTI2023

Atomic-scale identification of defects in alite

Crystallographic defects play a crucial role in cement hydration, with initial dissolution being dominated by the formation of etch pits that rely on the intersection of defects on surfaces. However, the defects present in cement particles have remained a mystery due to the lack of detailed direct observation at the atomic scale. In this study, we used scanning transmission electron microscopy to unravel the defects in alite particles at the single-atom level. Our observations identified different types of defects, including vacancies, doping, dislocations, rough surfaces, and grain boundaries. Atomic ordering in the alite crystal was further examined based on our single-atom recognition method. Our findings indicate that defects in cement particles may serve as reactive sites during the early hydration stage, facilitating the initial dissolution and providing nucleation sites for hydration products. Finally, this work provides insights into cement defect formation at the single-atom level and offers new opportunities in tuning the hydration process through defect engineering of cement particles.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Constraining Interlayer Slipping in P2-Type Layered Oxides with Oxygen Redox by Constructing Strong Covalent Bonds

Lattice oxygen redox (LOR) in P2-type layered oxides is an effective strategy to break through the limit of energy density of conventional cathodes due to its high redox potential (>4 V vs. Na + /Na) as well as extra capacity. Nevertheless, LOR induced local structure distortion and irreversible phase transitions cause serious electrochemical performance degradation, hindering the practical applications. In this work, we propose that the generation of the OP4 phase can be replaced with the Z phase by introducing Sb element with higher ionic potential and strong covalent bonds within the TMO 6 octahedron. Z phase transition is realized by constraining interlayer slipping between adjacent TM layers compared to OP4, which reduces the strain in the layered structure, lowers the Na+ diffusion energy barrier and creates more efficient Na+ diffusion channels. Consequently, Sb-substituted oxides demonstrates excellent kinetics, rate capability (79 mAh g -1 at 1 A g -1 ) in half cell and a high energy density of 487 Wh kg -1 (on cathode) in full cell.

25 ENERGY STORAGE↗
DOE OSTI2021

A capillary-based microfluidic device enables primary high-throughput room-temperature crystallographic screening

A novel capillary-based microfluidic strategy to accelerate the process of small-molecule-compound screening by room-temperature X-ray crystallography using protein crystals is reported. The ultra-thin microfluidic devices are composed of a UV-curable polymer, patterned by cleanroom photolithography, and have nine capillary channels per chip. The chip was designed for ease of sample manipulation, sample stability and minimal X-ray background. 3D-printed frames and cassettes conforming to SBS standards are used to house the capillary chips, providing additional mechanical stability and compatibility with automated liquid- and sample-handling robotics. These devices enable an innovative in situ crystal-soaking screening workflow, akin to high-throughput compound screening, such that quantitative electron density maps sufficient to determine weak binding events are efficiently obtained. This work paves the way for adopting a room-temperature microfluidics-based sample delivery method at synchrotron sources to facilitate high-throughput protein-crystallography-based screening of compounds at high concentration with the aim of discovering novel binding events in an automated manner.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Electrical conductivity of multilayered Cu/Nb composites fabricated by accumulative roll bonding

The electrical conductivity of nanolayered copper/niobium composites fabricated using accumulative roll bonding was investigated as a function of layer thickness. Cu/Nb was used as a model system to evaluate the processing-structure–property relationship stemming from the accumulative roll bonding process. The physical properties were compared against samples of individual average layer heights ranging from 193 to 25 nm. The electrical resistivity was measured over a temperature range of ~3–300 K. Analysis on the role of interfaces on temperature dependence is conducted including the residual resistivity ratio and temperature coefficient of resistivity. It was found that electrical resistivity increases with decreasing layer height.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Phase transformations and thermal expansion coefficients of unirradiated U-X wt.% Zr (X = 6, 10, 20, 30) measured via neutron diffraction

This work characterizes the crystallographic evolution of unirradiated U-X wt.% Zr (X = 6, 10, 20, 30) while cooling from equilibration, single phase γ-U-Zr, at 900 °C to ambient temperature using time-of-flight neutron diffraction. The β-U phase was unobserved during cooling at 1 °C/min in all alloys. All alloys followed the phase transformation pathway of γ-U-Zr→γ-U-Zr+α-U→α-U +δ-UZr2 with an observed miscibility gap in γ-U-Zr. The α-U and δ-UZr2 transformation took place simultaneously in the U-30 wt.% Zr sample. These findings strengthen the need to re-approach the U-Zr phase diagram in entirety. Bulk volumetric CTEs agree well with published data, strengthening the quantification of lattice-specific CTEs reported in this study. A compositionally dependent discontinuity in thermal expansion, increasing in magnitude with decreasing U content, occurs during the γ-U-Zr→α-U+δ-UZr2 transformation. The γ-U-Zr lattice parameter was measured to have a compositional dependency.

36 MATERIALS SCIENCE↗