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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Plant metacaspase: A case study of microcrystal structure determination and analysis

Metacaspases are highly conserved in plants and play essential roles in mediating programmed cell death, biotic and abiotic stress responses, and damage-induced innate immunity. Ca 2+ signaling induced by plant damage leads to activation of metacaspase from Arabidopsis thaliana (AtMC4), which subsequently processes a plant elicitor peptide to trigger downstream immuno-response. To understand the structural basis of AtMC4 activation by Ca 2+ , we previously determined its crystal structure and performed in-crystal Ca 2+ treatment to probe activation-associated conformational changes. To enable structure determination and in-crystal Ca 2+ activation analysis, we used microcrystals and related methods which were essential for our successful approach. Here, in this paper, we describe in detail the methods that we used for determination of AtMC4 structure using single-wavelength isomorphous replacement with anomalous signals assembled from 22 microcrystals. We also describe the method for in-crystal Ca 2+ soaking, microcrystal data collection, data assembly and analysis to obtain the activated structure of AtMC4 from 91 micro-sized crystals. The described methods may be useful to study other plant metacaspases and more broadly other plant enzymes for their structure determination and in-crystal functional characterization.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2012

Octahedral iron phosphate hydroxide microcrystals: Fast microwave-hydrothermal preparation, influencing factors and the shape evolution

Graphical abstract: Octahedral Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} microcrystals have been successfully prepared by a microwave-assisted hydrothermal route at 170 °C for 20 min. The morphology of Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} could be tuned by the Na{sub 2}SO{sub 3}/HAc molar ratio. Highlights: ► Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} octahedra had been hydrothermally prepared under the microwave assistance. ► The morphology of the final product could be tuned by the original molar ratio of Na{sub 2}SO{sub 3}/HAc. ► Low or high temperatures were unfavorable for the formation of Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} octahedra. ► The time-dependent shape evolution of the final product was investigated. -- Abstract: Octahedral Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} microcrystals have been successfully prepared by a microwave-assisted hydrothermal route at 170 °C for 20 min, employing FeCl{sub 3}·6H{sub 2}O and NaH{sub 2}PO{sub 4}·2H{sub 2}O as the starting materials in the presence of proper amounts of Na{sub 2}SO{sub 3} and acetic acid (HAc). The phase and morphology of the as-prepared product were characterized by means of powder X-ray diffraction (XRD), energy dispersive spectrometry (EDS), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Some factors influencing the formation of octahedral Fe{sub 4}(PO{sub 4}){sub 3}(OH){sub 3} microcrystals were systematically investigated, including the reaction temperature, time, and the molar ratio of Na{sub 2}SO{sub 3}/HAc.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Highly uniform YF{sub 3}:Ln{sup 3+} (Ln = Ce{sup 3+}, Tb{sup 3+}) walnut-like microcrystals: Hydrothermal synthesis and luminescent properties

Graphical abstract: The emission spectra of Y{sub 0.98−x}F{sub 3}:0.02Ce{sup 3+}, xTb{sup 3+} microcrystals with different Tb{sup 3+} concentrations demonstrated that energy transfer from the Ce{sup 3+} and Tb{sup 3+} ions is highly efficient. The concentration quenching phenomenon occurs when the x = 0.13. We have discussed it in detail based on experiments and quantitative calculations. Highlights: ► YF{sub 3}:Ce{sup 3+}, Tb{sup 3+} walnut-like microcrystals were prepared by a hydrothermal synthesis. ► The optical properties of YF{sub 3}:Ce{sup 3+}, Tb{sup 3+} phosphors have been investigated in detail. ► The energy transfer distance and efficiency from Ce{sup 3+} to Tb{sup 3+} ions were calculated. ► The dipole–dipole interaction should be the dominant mechanism for energy transfer. - Abstract: Uniform and well-crystallized YF{sub 3} walnut-like microcrystals were prepared by a facile one-step hydrothermal synthesis. The crystalline phase, size, morphology, and luminescence properties were characterized using powder X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), photoluminescence (PL) and photoluminescent excitation spectra (PLE). The results revealed that the existence of Ce{sup 3+} (sensitizer) can dramatically enhance green emission centered at 545 nm of Tb{sup 3+} (activator) in codoped samples due to an efficient energy transfer from Ce{sup 3+} to Tb{sup 3+}. The critical energy transfer distance between Ce{sup 3+} and Tb{sup 3+} was also calculated by methods of concentration quenching and spectral overlapping. Experimental analysis and theoretical calculations indicated that the dipole–dipole interaction should be the dominant mechanism for the Ce{sup 3+}–Tb{sup 3+} energy transfer.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Acoustically Mounted Microcrystals Yield High-Resolution X-ray Structures

We demonstrate a general strategy for determining structures from showers of microcrystals. It uses acoustic droplet ejection to transfer 2.5 nL droplets from the surface of microcrystal slurries, through the air, onto mounting micromesh pins. Individual microcrystals are located by raster-scanning a several-micrometer X-ray beam across the cryocooled micromeshes. X-ray diffraction data sets merged from several micrometer-sized crystals are used to determine 1.8 {angstrom} resolution crystal structures.

58 GEOSCIENCES↗
DOE OSTI2014

Three-dimensional periodic supramolecular organic framework ion sponge in water and microcrystals

Self-assembly has emerged as a powerful approach to generating complex supramolecular architectures. Despite there being many crystalline frameworks reported in the solid state, the construction of highly soluble periodic supramolecular networks in a three-dimensional space is still a challenge. In this paper we demonstrate that the encapsulation motif, which involves the dimerization of two aromatic units within cucurbit[8]uril, can be used to direct the co-assembly of a tetratopic molecular block and cucurbit[8]uril into a periodic three-dimensional supramolecular organic framework in water. The periodicity of the supramolecular organic framework is supported by solution-phase small-angle X-ray-scattering and diffraction experiments. Upon evaporating the solvent, the periodicity of the framework is maintained in porous microcrystals. Lastly, as a supramolecular 'ion sponge', the framework can absorb different kinds of anionic guests, including drugs, in both water and microcrystals, and drugs absorbed in microcrystals can be released to water with selectivity.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Structural Dynamics of GaN Microcrystals in Evolutionary Selection Selective Area Growth probed by X-ray Microdiffraction

A method to grow high quality, single crystalline semiconductor material irrespective of the substrate would allow a cost-effective improvement to functionality and performance of optoelectronic devices. Recently, a novel type of substrate-insensitive growth process called Evolutionary Selection Selective Area Growth (ES-SAG) has been proposed. Here we report the use of X-ray microdiffraction to study the structural properties of GaN microcrystals grown by ES-SAG. Utilizing high resolution in both direct and reciprocal spaces, we have unraveled structural dynamics of GaN microcrystals in growth structures of different dimensions. It has been found that the geometric proportions of the growth constrictions play an important role: 2.6 mm and 4.5 mm wide growth tunnels favor the evolutionary selection mechanism, contrary to the case of 8.6 mm growth tunnels. It was also found that GaN microcrystal ensembles are dominated by slight tensile strain irrespective of growth tunnel shape.

CHARACTERIZATION AND ANALYTICAL TECHNIQUES↗
DOE OSTI2015

Growth of very large InN microcrystals by molecular beam epitaxy using epitaxial lateral overgrowth

Very thick InN (∼40 μm) was grown by molecular beam epitaxy using the epitaxial lateral overgrowth (ELO) technique. In some regions, the ELO of InN was observed as expected, indicating an important step toward fabricating quasi-bulk InN substrates. Interestingly, most parts of the sample consist of large flat-topped microcrystals and well-faceted microstructures. This is likely due to local growth condition variations during ELO, which is supported by an experiment where ELO of InN was performed on a substrate with various stripe mask patterns. TEM characterization of a flat top InN microcrystal revealed few stacking faults and only related threading dislocations. Defect-free small faceted microcrystals were also observed. The thick InN crystals show a narrow photoluminescence spectrum with a peak at 0.679 eV and linewidth of 16.8 meV at 4 K.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Microcrystal manipulation with laser tweezers

Optical trapping has successfully been applied to select and mount microcrystals for subsequent X-ray diffraction experiments. X-ray crystallography is the method of choice to deduce atomic resolution structural information from macromolecules. In recent years, significant investments in structural genomics initiatives have been undertaken to automate all steps in X-ray crystallography from protein expression to structure solution. Robotic systems are widely used to prepare crystallization screens and change samples on synchrotron beamlines for macromolecular crystallography. The only remaining manual handling step is the transfer of the crystal from the mother liquor onto the crystal holder. Manual mounting is relatively straightforward for crystals with dimensions of >25 µm; however, this step is nontrivial for smaller crystals. The mounting of microcrystals is becoming increasingly important as advances in microfocus synchrotron beamlines now allow data collection from crystals with dimensions of only a few micrometres. To make optimal usage of these beamlines, new approaches have to be taken to facilitate and automate this last manual handling step. Optical tweezers, which are routinely used for the manipulation of micrometre-sized objects, have successfully been applied to sort and mount macromolecular crystals on newly designed crystal holders. Diffraction data from CPV type 1 polyhedrin microcrystals mounted with laser tweezers are presented.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Comparing serial X-ray crystallography and microcrystal electron diffraction (MicroED) as methods for routine structure determination from small macromolecular crystals

Innovative new crystallographic methods are facilitating structural studies from ever smaller crystals of biological macromolecules. In particular, serial X-ray crystallography and microcrystal electron diffraction (MicroED) have emerged as useful methods for obtaining structural information from crystals on the nanometre to micrometre scale. Despite the utility of these methods, their implementation can often be difficult, as they present many challenges that are not encountered in traditional macromolecular crystallography experiments. Here, XFEL serial crystallography experiments and MicroED experiments using batch-grown microcrystals of the enzyme cyclophilin A are described. The results provide a roadmap for researchers hoping to design macromolecular microcrystallography experiments, and they highlight the strengths and weaknesses of the two methods. Specifically, we focus on how the different physical conditions imposed by the sample-preparation and delivery methods required for each type of experiment affect the crystal structure of the enzyme.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Synthesis of monodispersed hierarchical Yb(OH){sub x}F{sub 3−x} microcrystals and their conversion to Yb{sub 6}O{sub 5}F{sub 8}

Highlights: • Monodispersed hierarchical Yb(OH){sub x}F{sub 3−x} microcrystals assembled by nanorod arrays were synthesized. • Yb(OH){sub x}F{sub 3−x} can be transformed to Yb{sub 6}O{sub 5}F{sub 8} with the retention of morphology. • Crystallographic relationship between Yb(OH){sub x}F{sub 3−x} and Yb{sub 6}O{sub 5}F{sub 8} and their transformation mechanism were disclosed. - Abstract: The fabrication of rare earth luminescent materials with monodispersed and hierarchical morphology is of great importance due to their various applications. In this report, monodispersed hierarchical Yb(OH){sub x}F{sub 3−x} microcrystals assembled by nanorod arrays were synthesized by a mild hydrothermal route. Calcination of Yb(OH){sub x}F{sub 3−x} resulted in the formation of Yb{sub 6}O{sub 5}F{sub 8} with the retention of morphology. The crystallographic structure relationship between Yb(OH){sub x}F{sub 3−x} and Yb{sub 6}O{sub 5}F{sub 8} and the transformation mechanism from Yb(OH){sub x}F{sub 3−x} to Yb{sub 6}O{sub 5}F{sub 8} were disclosed. The upconversion emission properties of the Er{sup 3+} doped samples were investigated. It can be found that Yb{sub 6}O{sub 5}F{sub 8}: 5%Er{sup 3+} exhibited an intense red light upconversion emission with the strongest peaks around 658 nm while Yb(OH){sub x}F{sub 3−x}: 5%Er{sup 3+} shows no upconversion emission.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Photo-actuators via epitaxial growth of microcrystal arrays in polymer membranes

Photomechanical crystals composed of three-dimensionally ordered and densely packed photochromes hold promise for high-performance photochemical actuators. However, bulk crystals with high structural ordering are severely limited in their flexibility, resulting in poor processibility and a tendency to fragment upon light exposure, while previous nano- or microcrystalline composites have lacked global alignment. Here we demonstrate a photon-fuelled macroscopic actuator consisting of diarylethene microcrystals in a polyethylene terephthalate host matrix. These microcrystals survive large deformations and show a high degree of three-dimensional ordering dictated by the anisotropic polyethylene terephthalate, which critically also has a similar stiffness. Overall, these ordered and compliant composites exhibit rapid response times, sustain a performance of over at least hundreds of cycles and generate work densities exceeding those of single crystals. In conclusion, our composites represent the state-of-the-art for photochemical actuators and enable properties unattainable by single crystals, such as controllable, reversible and abrupt jumping (photosalient behaviour).

36 MATERIALS SCIENCE↗
DOE OSTI2022

In situ Bragg coherent X-ray diffraction imaging of corrosion in a Co–Fe alloy microcrystal

Corrosion is a major concern for many industries, as corrosive environments can induce structural and morphological changes that lead to material dissolution and accelerate material failure. The progression of corrosion depends on nanoscale morphology, stress, and defects present. Experimentally monitoring this complex interplay is challenging. Here we implement in situ Bragg coherent X-ray diffraction imaging (BCDI) to probe the dissolution of a Co-Fe alloy microcrystal exposed to hydrochloric acid (HCl). By measuring five Bragg reflections from a single isolated microcrystal at ambient conditions, we compare the full three-dimensional (3D) strain state before corrosion and the strain along the [111] direction throughout the corrosion process. We find that the strained surface layer of the crystal dissolves to leave a progressively less strained surface. Interestingly, the average strain closer to the centre of the crystal increases during the corrosion process. We determine the localised corrosion rate from BCDI data, revealing the preferential dissolution of facets more exposed to the acid stream, highlighting an experimental geometry effect. These results bring new perspectives to understanding the interplay between crystal strain, morphology, and corrosion; a prerequisite for the design of more corrosion-resistant materials.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Time-resolved photoluminescence properties of semiconductor quantum dot superlattices of different microcrystal shapes

We report time-resolved photoluminescence properties on semiconductor quantum dot (QD) superlattices (SLs) using PL lifetime imaging microscopy at a single particle level. PL lifetime imaging technique clearly reveals that different shaped QD SL microcrystals have different time-resolved PL characteristics. The faceted SL microcrystals consisted of well-organized QDs showed faster recombination rates than those of the spherical microparticles including randomly organized QDs, which can be explained by the different degree of energetic couplings among component QDs due to different packing fraction.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Low-temperature state in strontium titanate microcrystals using in situ multireflection Bragg coherent x-ray diffraction imaging

Strontium titanate is a classic quantum paraelectric oxide material that has been widely studied in bulk and thin films. It exhibits a well-known cubic-to-tetragonal antiferrodistortive phase transition at 105 K, characterized by the rotation of oxygen octahedra. A possible second phase transition at lower temperature is suppressed by quantum fluctuations, preventing the onset of ferroelectric order. However, recent studies have shown that ferroelectric order can be established at low temperatures by inducing strain and other means. Here, we used in situ multireflection Bragg coherent x-ray diffraction imaging to measure the strain and rotation tensors for two strontium titanate microcrystals at low temperature. We observe strains induced by dislocations and inclusion-like impurities in the microcrystals. Based on radial magnitude plots, these strains increase in magnitude and spread as the temperature decreases. Pearson's correlation heat maps show a structural transition at 50 K, which could possibly be the formation of a low-temperature ferroelectric phase in the presence of strain. We do not observe any change in local strains associated with the tetragonal phase transition at 105 K.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Serial femtosecond X-ray diffraction of 30S ribosomal subunit microcrystals in liquid suspension at ambient temperature using an X-ray free-electron laser

High-resolution ribosome structures determined by X-ray crystallography have provided important insights into the mechanism of translation. Such studies have thus far relied on large ribosome crystals kept at cryogenic temperatures to reduce radiation damage. Here, the application of serial femtosecond X-ray crystallography (SFX) using an X-ray free-electron laser (XFEL) to obtain diffraction data from ribosome microcrystals in liquid suspension at ambient temperature is described. 30S ribosomal subunit microcrystals diffracted to beyond 6 Å resolution, demonstrating the feasibility of using SFX for ribosome structural studies. The ability to collect diffraction data at near-physiological temperatures promises to provide fundamental insights into the structural dynamics of the ribosome and its functional complexes.

30S ribosomal subunit↗
DOE OSTI2017

Serial millisecond crystallography of membrane and soluble protein microcrystals using synchrotron radiation

Crystal structure determination of biological macromolecules using the novel technique of serial femtosecond crystallography (SFX) is severely limited by the scarcity of X-ray free-electron laser (XFEL) sources. However, recent and future upgrades render microfocus beamlines at synchrotron-radiation sources suitable for room-temperature serial crystallography data collection also. Owing to the longer exposure times that are needed at synchrotrons, serial data collection is termed serial millisecond crystallography (SMX). As a result, the number of SMX experiments is growing rapidly, with a dozen experiments reported so far. Here, the first high-viscosity injector-based SMX experiments carried out at a US synchrotron source, the Advanced Photon Source (APS), are reported. Microcrystals (5–20 µm) of a wide variety of proteins, including lysozyme, thaumatin, phycocyanin, the human A 2A adenosine receptor (A 2A AR), the soluble fragment of the membrane lipoprotein Flpp3 and proteinase K, were screened. Crystals suspended in lipidic cubic phase (LCP) or a high-molecular-weight poly(ethylene oxide) (PEO; molecular weight 8 000 000) were delivered to the beam using a high-viscosity injector. In-house data-reduction (hit-finding) software developed at APS as well as the SFX data-reduction and analysis software suites Cheetah and CrystFEL enabled efficient on-site SMX data monitoring, reduction and processing. Complete data sets were collected for A 2A AR, phycocyanin, Flpp3, proteinase K and lysozyme, and the structures of A 2A AR, phycocyanin, proteinase K and lysozyme were determined at 3.2, 3.1, 2.65 and 2.05 Å resolution, respectively. The data demonstrate the feasibility of serial millisecond crystallography from 5–20 µm crystals using a high-viscosity injector at APS. The resolution of the crystal structures obtained in this study was dictated by the current flux density and crystal size, but upcoming developments in beamline optics and the planned APS-U upgrade will increase the intensity by two orders of magnitude. Furthermore, these developments will enable structure determination from smaller and/or weakly diffracting microcrystals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

The Structure of Radiative Tunnel Recombination Sites in Emulsion Microcrystals of AgBr(I)

To identify the structure of emissive tunnel recombination sites in the emulsion microcrystals of silver bromide AgBr(I) with iodine contaminations and to determine the role of an emulsion medium in their formation, the temperature dependence of the luminescence spectra in the range from 77 to 120 K, the kinetics of the growth of the maximum luminescence intensity value at λ ≈ 560 nm, and the luminescence flash spectrum stimulated by the infrared light are investigated. Two types of the AgBr{sub 1–} {sub x}(I{sub x}) (x = 0.03) microcrystals—namely, obtained in an aqueous solution and on a gelatin substrate—are used in the studies. It is established that the emissive tunnel recombination sites with a luminescence maximum at λ ≈ 560 nm in AgBr{sub 1–} {sub x}(I{sub x}) (x = 0.03) are the {(I_a"-I_a"-)Ag_i"+} donor–acceptor complexes with the I{sub a}{sup -} iodine ions located in neighbor anionic sites of the AgBr(I) crystal lattice, next to which the Ag{sub i}{sup +} interstitial silver ion is positioned. With an increase in the temperature, the {(I_a"-I_a"-)Ag_i"+} sites undergo structural transformation into the {(I_a"-I_a"-)Ag_i_n"+} sites, where n = 2, 3, …. Moreover, the {(I_a"-I_a"-)Ag_i_n"+} sites (n = 2) after the capture of an electron and hole also provide the tunnel recombination with a luminescence maximum at λ ≈ 720 nm. The influence of an emulsion medium consists in that gelatin interacts with the surface electron-localization sites, i.e., the interstitial silver ions Ag{sub in}{sup +}, n = 1, 2, and forms the complexes {Ag_i_n"0 G"+} (n = 1, 2) with them. The latter are deeper electron traps with a small capture cross section as compared to the Ag{sub in}{sup +} sites (n = 1, 2) and that manifest themselves in that the kinetics of the luminescence growth in AgBr(I) to a stationary level at λ ≈ 560 nm is characterized by the presence of “flash firing.” At the same time, the luminescence flash stimulated by IR light, for which the Ag{sub in}{sup +}(n = 1, 2) electron-localization sites are responsible, is absent. It is supposed that the electrons localized on the {Ag_i_n"+G"+} complexes (n = 2) retain the capability for emissive tunnel recombination with holes localized on paired iodine sites with a luminescence maximum at λ ≈ 750 nm.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Serial Femtosecond X-Ray Diffraction of HIV-1 Gag MA-IP6 Microcrystals at Ambient Temperature

The Human immunodeficiency virus-1 (HIV-1) matrix (MA) domain is involved in the highly regulated assembly process of the virus particles that occur at the host cell’s plasma membrane. High-resolution structures of the MA domain determined using cryo X-ray crystallography have provided initial insights into the possible steps in the viral assembly process. However, these structural studies have relied on large and frozen crystals in order to reduce radiation damage caused by the intense X-rays. Here, we report the first X-ray free-electron laser (XFEL) study of the HIV-1 MA domain’s interaction with inositol hexaphosphate (IP6), a phospholipid headgroup mimic. We also describe the purification, characterization and microcrystallization of two MA crystal forms obtained in the presence of IP6. In addition, we describe the capabilities of serial femtosecond X-ray crystallography (SFX) using an XFEL to elucidate the diffraction data of MA-IP6 complex microcrystals in liquid suspension at ambient temperature. Two different microcrystal forms of the MA-IP6 complex both diffracted to beyond 3.5 Å resolution, demonstrating the feasibility of using SFX to study the complexes of MA domain of HIV-1 Gag polyprotein with IP6 at near-physiological temperatures. Further optimization of the experimental and data analysis procedures will lead to better understanding of the MA domain of HIV-1 Gag and IP6 interaction at high resolution and will provide basis for optimization of the lead compounds for efficient inhibition of the Gag protein recruitment to the plasma membrane prior to virion formation.

59 BASIC BIOLOGICAL SCIENCES↗