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At least 1,657 records · Page 92
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Large-volume protein crystal growth for neutron macromolecular crystallography

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for the growth of crystals to significant dimensions that are now relevant to NMC are revisited. We report that these include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Preparing for successful protein crystallization experiments

Crystal-based structural methods, including X-ray crystallography, are frequently utilized for the determination of high-resolution structures of biomolecules. All crystal-based diffraction methods first require the preparation of biomolecular crystals, and careful sample preparation for crystallization experiments can increase the frequency of success. In this article, strategies to optimize factors that can impact crystallization are presented, from which buffers and reducing agents are most favorable to which crystallization techniques could be used.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Crystal structures and comparisons of huntite aluminum borates RE Al 3 (BO 3 ) 4 ( RE = Tb, Dy and Ho)

Three huntite-type aluminoborates of stoichiometry RE Al 3 (BO 3 ) 4 ( RE = Tb, Dy and Ho), namely, terbium/dysprosium/holmium trialuminium tetrakis(borate), were synthesized by slow cooling within a K 2 Mo 3 O 10 flux with spontaneous crystallization. The crystal structures were determined using single-crystal X-ray diffraction (SC-XRD) data. The synthesized borates are isostructural to the huntite [CaMg 3 (CO 3 ) 4 ] structure and crystallized within the trigonal R 32 space group. The structural parameters were compared to literature data of other huntite RE Al 3 (BO 3 ) 4 crystals within the R 32 space group. All three borates fit well into the trends calculated from the literature data. The unit-cell parameters and volumes increase linearly with larger RE cations whereas the densities decrease. All of the crystals studied were refined as inversion twins.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Effect of stacking sequence on crystallization in Al/a-Ge bilayer thin films

Two types of bilayer thin films with different deposition sequences, i.e., amorphous Ge under Al (a-Ge/Al) and the inverse (Al/a-Ge), were prepared by magnetron sputtering at room temperature. In-situ and ex-situ thermal annealing were compared to study the effect of the stacking sequence on crystallization of amorphous Ge. Although metal-induced crystallization occurred in both cases at low temperature, layer exchange was observed only in a-Ge/Al. In fact, compressive stress could usually be produced when Ge atoms diffused into Al grain boundaries and crystallized there. In the a-Ge/Al system, the stress could be released through diffusion of Al atoms onto the surface and formation of hillocks. Thus, grain boundary (GB) mediated crystallization was dominant in the whole process and layer exchange occurred. However, in the Al/a-Ge system, it was difficult for stress to be relaxed because the Ge sublayer and substrate restricted the diffusion of Al atoms. GB-mediated crystallization was, therefore, considerably suppressed and interface-mediated crystallization was preferred without layer exchange. This leads to distinct morphologies of dendrites in the two systems.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Effect of H{sup +} implantation on the optical properties of semi-insulating GaAs crystals in the IR spectral region

The optical properties of semi-insulating GaAs crystals subjected to multienergy hydrogen-ion implantation and treatment in a high-frequency electromagnetic field are studied in the infrared spectral region. It is established that such combined treatment provides a means for substantially increasing the transmittance of GaAs crystals to values characteristic of crystals of high optical quality. On the basis of analysis of the infrared transmittance and reflectance data, Raman spectroscopy data, and atomic-force microscopy data on the surface morphology of the crystals, a physical model is proposed to interpret the effects experimentally observed in the crystals. The model takes into account the interaction of radiation defects with the initial structural defects in the crystals as well as the effect of compensation of defect centers by hydrogen during high-frequency treatment.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Bulk-Density Representations of Branched Planar Ice Crystals: Errors in the Polarimetric Radar Variables

Abstract Recent interest in interpreting polarimetric radar observations of ice and evaluating microphysical model output with these observations has highlighted the importance of accurately computing the scattering of microwave radiation by branched planar ice crystals. These particles are often represented as spheroids with uniform bulk density, reduced from that of solid ice to account for the complex, nonuniform structure of natural branched crystals. In this study, the potential errors that arise from this assumption are examined by comparing scattering calculations of branched planar crystals with those of homogeneous, reduced-density plate crystals and spheroids with the same mass, aspect ratio, and maximum dimension. The results show that this assumption leads to significant errors in backscatter cross sections at horizontal and vertical polarization, specific differential phase (KDP), and differential reflectivity (ZDR), with the largest ZDR errors for ice crystals with the most extreme aspect ratios (<0.01) and effective densities < 250 kg m−3. For example, the maximum errors in X-band ZDR are 4.5 dB for 5.6-mm branched planar crystals. However, substantial errors are present at all weather radar frequencies, with resonance scattering effects at Ka and W band amplifying the low-frequency errors. The implications of these results on the interpretation of polarimetric radar observations and forward modeling of the polarimetric radar variables from microphysical model output are discussed.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2015

Event Localization in Bulk Scintillator Crystals Using Coded Apertures

The localization of radiation interactions in bulk scintillators is generally limited by the size of the light distribution at the readout surface of the crystal/light-pipe system. By finding the centroid of the light spot, which is typically of order centimeters across, practical single-event localization is limited to ~2 mm/cm of crystal thickness. Similar resolution can also be achieved for the depth of interaction by measuring the size of the light spot. Through the use of near-field coded-aperture techniques applied to the scintillation light, light transport simulations show that for 3-cm-thick crystals, more than a five-fold improvement (millimeter spatial resolution) can be achieved both laterally and in event depth. At the core of the technique is the requirement to resolve the shadow from an optical mask placed in the scintillation light path between the crystal and the readout. In this paper, experimental results are presented that demonstrate the overall concept using a 1D shadow mask, a thin-scintillator crystal and a light pipe of varying thickness to emulate a 2.2-cm-thick crystal. Spatial resolutions of ~ 1 mm in both depth and transverse to the readout face are obtained over most of the crystal depth.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Hydrothermal Growth of Magnetically Frustrated Crystals: Lanthanide Stannate Pyrochlores as a Prototype

One important test bed system for frustrated magnetism is the pyrochlore lattice with the formula A2B2O7 in the cubic space group Fd3(-)m. Both the A and B sites occupy crystallographic trigonal sites and both sites possess a tetrahedral relationship with the other similar metal ion sites. These symmetry relationships generate a 3 D frustrated structure. In frustrated magnetic systems, typically a trivalent lanthanide ion occupies the A site and a magnetically silent tetravalent ion (Ti, Zr, Sn, etc.) occupies the B site. A classical problem related to the crystal growth of these compounds is sample quality. As refractory oxides, the traditional synthesis and crystal growth techniques require high temperatures, which creates two problems that are quite common and endemic to the pyrochlores. One is oxide lattice defects and the other is A/B site disorder. Both issues often occur in the same crystals at the same time and can have a significant impact on the study of physical properties. A hydrothermal approach can be applied to this problem. The relatively low crystal growth temperatures (600-720˚C) greatly minimize nonstoichiometry, lattice defects and A/B site disorder. The reduction of these pervasive imperfections significantly increases the quality of the observed physical property data. This talk will focus on the lanthanide stannates Ln2Sn2O7 as a prototype test bed of these systems. The stannates are among the few building blocks that can stabilize the pyrochlore structure type for all the lanthanides and they serve as an excellent proving ground for a wide range of physical properties. The synthesis and crystal growth of the lanthanide stannates will be reviewed, along with a discussion of some of the physical properties that result from the frustrated magnetic states of these low defect crystals.

Hydrothermal, crystal growth↗
DOE OSTI2023

Structural and Improper Ferroelectric Properties of TbInO 3 Single Crystal Grown by Laser Floating Zone

The honeycomb TbInO 3 has attracted wide research attention due to its fascinating physical properties. However, TbInO 3 single crystal was difficult to grow owing to the high melting point and serious volatilization of indium during the crystal growth. In this study, the volatilization of the indium element was effectively suppressed by controlling the growth atmosphere and pressure. The excess ratio of indium oxide was determined, and pure hexagonal TbInO 3 crystal was obtained by the laser floating zone method. Systematic studies on the crystal structure and optical and ferroelectric properties were carried out. The structure distortion resulted in the improper geometric ferroelectric revealed by single crystal diffraction and Raman spectrum measurements. The topological vortex domains and P-E hysteresis loop demonstrated the presence of ferroelectricity. TbInO 3 crystal has great potential application in vortex memory.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Getting the Most Out of Your Crystals: Data Collection at the New High-Flux, Microfocus MX Beamlines at NSLS-II

Advances in synchrotron technology are changing the landscape of macromolecular crystallography. The two recently opened beamlines at NSLS-II—AMX and FMX—deliver high-flux microfocus beams that open new possibilities for crystallographic data collection. They are equipped with state-of-the-art experimental stations and automation to allow data collection on previously intractable crystals. Optimized data collection strategies allow users to tailor crystal positioning to optimally distribute the X-ray dose over its volume. Vector data collection allows the user to define a linear trajectory along a well diffracting volume of the crystal and perform rotational data collection while moving along the vector. This is particularly well suited to long, thin crystals. We describe vector data collection of three proteins—Akt1, PI3Kα, and CDP-Chase—to demonstrate its application and utility. For smaller crystals, we describe two methods for multicrystal data collection in a single loop, either manually selecting multiple centers (using H108A-PHM as an example), or “raster-collect”, a more automated approach for a larger number of crystals (using CDP-Chase as an example).

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS1999

Crystallization and preliminary X-ray diffraction analysis of restriction endonuclease EcoRII

Crystals of the restriction endonuclease EcoRII have been obtained by the vapor-diffusion technique in the presence of ammonium sulfate or polyethylene glycol. The best crystals were grown with ammonium sulfate as a precipitant. Crystals with dimensions of up to 0.6 x 0. 6 x 0.6 mm have been observed. The crystals diffract to about 4.0 A resolution at a cryo-temperature of 100 K using a rotating-anode X-ray source and a Rigaku R-AXIS IV imaging-plate detector. The space group has been determined to be either I23 or I2(1)3, with unit-cell parameters a = b = c = 160.3 A, alpha = beta = gamma = 90 degrees. The crystal asymmetric unit contains two protein molecules, and self-rotation function analysis shows a pseudo-twofold symmetry relating the two monomers. Attempts to improve the resolution of crystal diffraction and to search for heavy-atom derivatives are under way.

Deoxyribonucleases, Type II Site-Specific/chemistr↗
NASA NTRS2014

A Flexible Parameterization for Shortwave Optical Properties of Ice Crystals

A parameterization is presented that provides extinction cross section sigma (sub e), single-scattering albedo omega, and asymmetry parameter (g) of ice crystals for any combination of volume, projected area, aspect ratio, and crystal distortion at any wavelength in the shortwave. Similar to previous parameterizations, the scheme makes use of geometric optics approximations and the observation that optical properties of complex, aggregated ice crystals can be well approximated by those of single hexagonal crystals with varying size, aspect ratio, and distortion levels. In the standard geometric optics implementation used here, sigma (sub e) is always twice the particle projected area. It is shown that omega is largely determined by the newly defined absorption size parameter and the particle aspect ratio. These dependences are parameterized using a combination of exponential, lognormal, and polynomial functions. The variation of (g) with aspect ratio and crystal distortion is parameterized for one reference wavelength using a combination of several polynomials. The dependences of g on refractive index and omega are investigated and factors are determined to scale the parameterized (g) to provide values appropriate for other wavelengths. The parameterization scheme consists of only 88 coefficients. The scheme is tested for a large variety of hexagonal crystals in several wavelength bands from 0.2 to 4 micron, revealing absolute differences with reference calculations of omega and (g) that are both generally below 0.015. Over a large variety of cloud conditions, the resulting root-mean-squared differences with reference calculations of cloud reflectance, transmittance, and absorptance are 1.4%, 1.1%, and 3.4%, respectively. Some practical applications of the parameterization in atmospheric models are highlighted.

parameterization↗
NASA NTRS2024

Morphology and Luminescence Properties of Transition Metal Doped Zinc Selenide Crystals

Zinc selenide is an excellent matrix material to dope with rare-earth and transition metal to achieve mid-infrared luminescence to develop high power lasers. The luminescence, morphology and refractive index is significantly affected by the doping and defects generated due to size and valency of dopants, concentration, growth process and convection during the growth. The aim of the study is to investigate effect of point and line defects generated due to low doping of iron and chromium on the emission and morphology of the zinc selenide. Luminescence and morphological properties of large iron and chromium doped zinc selenide single crystals were studied to evaluate the effect of extremely low residual impurities and defects associated with the doping process. The emission properties following both short wavelength (i.e., ultraviolet; 350 – 370 nm) excitation and longer wavelength (i.e., near infrared; 850 – 870 nm) excitation were characterized. Luminescence emission bands were identified in both doped crystals. In addition to the primary emission bands, satellite peaks and intra-center transitions were also observed. Due to local population defects associated with the residual impurities (ppm to ppb) in the Fe-ZnSe and Cr-ZnSe crystals, peak emission wavelengths were observed to shift. Raman studies using 266 and 532 – nm excitation revealed different positions of longitudinal and transverse peaks for Fe-ZnSe and Cr-ZnSe crystals, associated with different levels of defects due to the different ion sizes. The emission bands were found to decrease in intensity due to recombination of residual impurity co-dopants and complex defects generated during growth and fabrication. Cryogenic temperature analyses revealed a very clean emission band due to freezing of some of the point and line defects. An emission band observed at 980 nm for both crystals at room temperature as well as cryogenic temperatures indicates a vibronic peak in ZnSe. The scanning electron microscopy (SEM) images of the local morphology support the conclusion that small crystallites in doped crystals are also present.

Zinc selenide↗
DOE OSTI2015

Determining the diffraction properties of a cylindrically bent KAP(001) crystal from 1 to 5 keV

Various crystals are used for the dispersive component of X-ray spectrometers. The crystals are usually bent to meet the desired measurement needs, such as focusing. The bending can change the crystal diffraction properties, thus altering the spectrometer throughput and resolving power. This work concerns measuring the diffraction properties of a potassium acid phthalate (001) [KAP(001)] crystal bent into a circular cylinder segment. The measurement methods using a diode source and a synchrotron source are described. The multi-lamellar model for calculating the diffraction properties of a bent crystal is described. The measurement results are compared to the multi-lamellar model and show qualitative agreement. The measurements show how to make the multi-lamellar calculations a useful estimate. A method is given to make useful estimates of the diffraction properties of the KAP(001) crystal bent into a circular cylinder segment.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Crystal Growth Scale-Up and Stability of RbSr 2 X 5 :Eu Scintillators

The discovery and development of new scintillation materials support national security needs. In these applications, large volumes of scintillator crystals are needed to achieve efficient screening for contraband. Therefore, one important step in the discovery of new scintillator compositions is testing their feasibility for scale-up and their stability. In this work, high-quality Ø22 mm crystals of two new scintillators RbSr 2 Br 5 :Eu and RbSr 2 I 5 :Eu were grown via the Vertical Bridgman method, and their scintillation properties were characterized. Here, the Ø22 mm RbSr 2 I 5 :Eu crystals could be grown with fast translation rates up to 3.5 mm/h. Both RbSr 2 Br 5 :Eu and RbSr 2 I 5 :Eu had high scintillation performance, including light yields of 46,000 and 61,000 ph/MeV, respectively, for Ø22 × 35 mm crystals. Additionally, properties related to physical stability were investigated, including the coefficients of thermal expansion via high-temperature X-ray diffraction (HTXRD) as well as moisture sensitivity. HTXRD confirmed the absence of solid–solid phase transitions and showed that RbSr 2 Br 5 had minimal thermal expansion anisotropy compared to RbSr 2 I 5 and some other inorganic metal halide scintillators, which favors the growth of large-sized crystals.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Influence of the Laser Scanning Rate on the Structure of Rotating Lattice Single Crystal Lines

Localized controlled heating of glass with a continuous wave laser has introduced the possibility of engineering the lattice of recently discovered rotating lattice single (RLS) crystals and thus obtaining novel metamaterials. On this account, we report the role of the laser scanning speed on the lattice structure of a model system: Sb 2 S 3 straight RLS crystal lines created in a 16SbI 3 -84Sb 2 S 3 glass. The electron backscatter diffraction analysis shows that above a critical laser scanning speed the lattice rotates along the direction of scanning, the rate of lattice rotation is relatively insensitive to scanning speed, and the growth front is symmetric. In contrast, for laser scanning speeds below this critical value, the rate and direction of lattice rotation are strongly affected by the speed. Further, the growth front becomes asymmetric, which promotes the formation of new grains misoriented by ≤10°. These observations are reported on in terms of the relative dominance of the temperature gradient from laser scanning vis-á-vis the intrinsic preferred crystallographic direction of crystal growth. In addition to providing guidelines for fabricating the RLS crystal of the desired rate of the lattice rotation, new insight is gained for the mechanism of plumose formation in spherulitic crystals.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Designing Sequence-Defined Peptoids for Biomimetic Control over Inorganic Crystallization

Crystallization defines what the world is all about, ranging from biomineralization in living organisms to various materials in our lives. During these processes, biomineralization set a superexcellent example of the additive-controlled crystallization. However, the high complexity and low stability of peptides and proteins preclude their wide applications in controlling inorganic crystallization beyond the biological systems. Peptoids are one type of sequence-defined biomimetic polymers with a simple structure, high stability, protein-like molecular recognition, and distinctive self-assembly properties. They provide a promising alternative to mimic peptides and proteins for controlling inorganic crystallization and extend its application to predictive materials synthesis. In this review article, we extract the main concepts of peptoid engineering and highlight the recent advances in peptoid-controlled inorganic crystallization. Our focus is to understand the principles of sequence engineering that lead to the predictable physiochemical properties of these substances, which will give insights into other inorganic systems.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Determination of crystal grain orientations by optical microscopy at textured surfaces

In this contribution, a new method to determine the crystal orientation with the example of chemical treated silicon wafers by means of optical microscopy has been demonstrated. The introduced procedure represents an easy method to obtain all relevant parameters to describe the crystal structure of the investigated material, i.e., the crystal grain orientation and the grain boundary character. The chemical treatment is a standard mono-texture for solar cells, well known in the solar industry. In general, this concept can also be applied to other crystalline materials, i.e., GaAs, SiC, etc., the only thing that needs to be adjusted is the texturing method to reveal specific crystal planes and the calculation model. In conclusion, an application of this method is shown with the example of the defect classification of recombination active defects in mc-Si solar cell. The introduced method demonstrates a simple and quick opportunity to improve the crystallization process and the quality of electronic devices by means of an optical microscope and a chemical treatment of the material.

14 SOLAR ENERGY↗