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At least 289 records · Page 16
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Wide-blocky veins explained by dependency of crystal growth rate on fracture surface type: Insights from phase-field modeling

Vein microstructures contain a wealth of information on coupled chemical and mechanical processes of fracturing, fluid transport, and crystal growth. Numerical simulations have been used for exploring the factors controlling the development of vein microstructures; however, they have not been quantitatively validated against natural veins. Here we combined phase-field modeling with microtextural analysis of previously unexplained wide-blocky calcite veins in natural limestone and of the fresh fracture surface in this limestone. Results show that the wide-blocky vein textures can only be reproduced if ~10%–20% of crystals grow faster than the rest. This fraction corresponds to the amount of transgranularly broken grains that were observed on the experimental fracture surfaces, which are dominantly intergranular. We hypothesize that transgranular fractures allow faster growth of vein minerals due to the lack of clay coatings and other nucleation discontinuities that are common along intergranular cracks. Our simulation results show remarkable similarity to the natural veins and reproduce the nonlinear relationship between vein crystal width and vein aperture. This allows accurate simulations of crystal growth processes and related permeability evolution in fractured rocks.

Geology↗
DOE OSTI2021

Toward In Situ Synchrotron Mapping of Crystal Selection Processes during Crystal Growth

In this work, we present an automated and rapid method for non-destructive mapping of crystal grains in a rod-shaped sample. The approach was designed for application to in situ float-zone crystal growth experiments at an x-ray synchrotron source, but could be useful in other applications. The methods have been tested on a TiO 2 boule grown in an optical float zone furnace. The approach applies a statistical filter to polycrystalline diffraction patterns on 2D detectors to rapidly determine the degree of powder-quality 1of the signal. When larger crystals emerge in the growth, their position, size and shape can be tracked using an automated blob-tracking algorithm that follows individual Bragg peaks as a function of position in a grid-scan, even when multiple crystals are contributing spots to diffraction images. This method is found to be robust as the same crystal shape can be independently reconstructed using different sets of Bragg reflections. Image segmentation methods are then used to map out the polycrystalline grains. We also note that other information about crystal quality, such as mosaicity or strain state, may be inferred and mapped from the intensity variation of the Bragg peaks at different locations within the sample.

36 MATERIALS SCIENCE↗
NASA NTRS1992

Continuing adventures in lysozyme crystal growth

Results obtained on the crystal nucleation and growth of lysozyme are presented. Special attention is given to the anion-protein binding, the nucleation kinetics, the mechanisms of aggregation, and the conditions that promote or inhibit lysozyme (110)-face growth rate. The emerging theory that is currently being used for data interpretation and for designing new experimental approaches is outlined.

Pusey, Marc L.↗
NASA NTRS1995

G-Jitter Effects in Protein Crystal Growth - A Numerical Study

The impact of spacecraft acceleration environment on Protein Crystal Growth (PCG) is studied. A brief overview of the Space Shuttle acceleration environment is provided followed by a simple scaling procedure used to obtain estimates of the flow and concentration field characteristics in PCG. A detailed two-dimensional numerical model is then used to simulate the PCG system response to different disturbance scenarios; viz. residual g effects, impulse type disturbances and oscillatory inputs. The results show that PCG is susceptible to g-jitter and is a good candidate for vibration isolation.

Ramachandran, N.↗
NASA NTRS2008

High-Temperature Crystal-Growth Cartridge Tubes Made by VPS

Cartridge tubes for use in a crystal growth furnace at temperatures as high as 1,600 deg. C have been fabricated by vacuum plasma spraying (VPS). These cartridges consist mainly of an alloy of 60 weight percent molybdenum with 40 weight percent rhenium, made from molybdenum powder coated with rhenium. This alloy was selected because of its high melting temperature (approximately equal.2,550 C) and because of its excellent ductility at room temperature. These cartridges are intended to supplant tungsten/nickel-alloy cartridges, which cannot be used at temperatures above approximately equal 1,300 C.

Holmes, Richard↗
NASA NTRS2003

Active Control of Interface Shape During the Crystal Growth of Lead Bromide

A thermal model for predicting and designing the furnace temperature profile was developed and used for the crystal growth of lead bromide. The model gives the ampoule temperature as a function of the furnace temperature, thermal conductivity, heat transfer coefficients, and ampoule dimensions as variable parameters. Crystal interface curvature was derived from the model and it was compared with the predicted curvature for a particular furnace temperature and growth parameters. Large crystals of lead bromide were grown and it was observed that interface shape was in agreement with the shape predicted by this model.

Duval, W. M. B.↗
NASA NTRS2004

Semiconductor Crystal Growth in Static and Rotating Magnetic fields

Magnetic fields have been applied during the growth of bulk semiconductor crystals to control the convective flow behavior of the melt. A static magnetic field established Lorentz forces which tend to reduce the convective intensity in the melt. At sufficiently high magnetic field strengths, a boundary layer is established ahead of the solid-liquid interface where mass transport is dominated by diffusion. This can have a significant effect on segregation behavior and can eliminate striations in grown crystals resulting from convective instabilities. Experiments on dilute (Ge:Ga) and solid solution (Ge-Si) semiconductor systems show a transition from a completely mixed convective state to a diffusion-controlled state between 0 and 5 Tesla. In HgCdTe, radial segregation approached the diffusion limited regime and the curvature of the solid-liquid interface was reduced by a factor of 3 during growth in magnetic fields in excess of 0.5 Tesla. Convection can also be controlled during growth at reduced gravitational levels. However, the direction of the residual steady-state acceleration vector can compromise this effect if it cannot be controlled. A magnetic field in reduced gravity can suppress disturbances caused by residual transverse accelerations and by random non-steady accelerations. Indeed, a joint program between NASA and the NHMFL resulted in the construction of a prototype spaceflight magnet for crystal growth applications. An alternative to the suppression of convection by static magnetic fields and reduced gravity is the imposition of controlled steady flow generated by rotating magnetic fields (RMF)'s. The potential benefits of an RMF include homogenization of the melt temperature and concentration distribution, and control of the solid-liquid interface shape. Adjusting the strength and frequency of the applied magnetic field allows tailoring of the resultant flow field. A limitation of RMF's is that they introduce deleterious instabilities above a critical magnetic field value. Growth conditions in which static magnetic fields rotational magnetic fields, and reduced gravitational levels can have a beneficial role will be described.

Volz, Martin↗
DOE OSTI2026

Crystal Growth of Quaternary RE 2 EuSi 2 S 8 ( RE = Ce–Nd, Sm, Gd, Tb) Using Flux-Assisted Boron Chalcogen Mixture (BCM) Method: Investigation of Magnetic and Luminescence Properties

A series of quaternary rare-earth containing thiosilicates with the general formula RE 2 EuSi 2 S 8 (RE = Ce–Nd, Sm, Gd, Tb) has been synthesized via the flux-assisted boron chalcogen mixture (BCM) crystal growth method. High-quality single crystals were obtained, and their crystal structures were determined by single-crystal X-ray diffraction. The RE 2 EuSi 2 S 8 series crystallizes in the trigonal system, adopting the space group R-3c. Polycrystalline samples were employed for physical property measurements, including magnetic susceptibility measurements, UV–visible diffuse reflectance, and photoluminescent response. Magnetic data of RE 2 EuSi 2 S 8 ( RE = Ce, Nd, and Gd) were collected over the 2–300 K temperature range. The samples were paramagnetic behavior with negative Weiss constants (θ W = −11.05, −10.55, and −1.35 K respectively). Their thermal stability was investigated using thermogravimetric analysis (TGA). Optical band gaps, estimated from diffuse reflectance spectra, were determined to be 2.2(1) eV for Ce 2 EuSi 2 S 8 , 1.8(1) eV for Nd 2 EuSi 2 S 8 , and 1.7(1) eV for Gd 2 EuSi 2 S 8 respectively. Finally, photoluminescence measurements were collected on Ce 2 EuSi 2 S 8 and Tb 2 EuSi 2 S 8 single crystals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1997

A Rationale for System-Dependent Advantages and Disadvantages of Solution Crystal Growth at Low Gravity

Protein crystallization experiments at reduced gravity have yielded crystals that, depending on the specific material, are either superior or inferior in their structural perfection compared to counterparts grown at normal gravity. A reduction of the crystals' quality due to their growth at low gravity cannot be understood from existing models. Our experimental investigations of the ground-based crystallization of the protein lysozyme have revealed pronounced unsteady growth layer dynamics and associated defect formation under steady external conditions. Through scaling analysis and numerical simulations we show that the observed fluctuations originate from the coupling of bulk transport with non-linear interface kinetics under mixed kinetics-transport control of the growth rate. The amplitude of the fluctuations is smallest when either transport or interfacial kinetics dominate the control of the crystallization process. Thus, depending on the specific system, crystal quality may be improved by either enhancing or suppressing the transport in the solution. These considerations provide, for the first time, a material-dependent rationale for the advantages, as well as the disadvantages, of reduced gravity for (protein) crystallization.

Rosenberger, Franz↗
NASA NTRS2001

Crystal Growth of HgZnTe Alloy by Directional Solidification in Low Gravity Environment

A Hg0.84Zn0.16Te alloy crystal was back-melted and partially resolidified during the first United States Microgravity Laboratory (USML-1) mission in the Marshall Space Flight Center's Crystal Growth Furnace. The experiment was inadvertently terminated at about 30% of planned completion. Nonetheless, it was successfully demonstrated that a HgZnTe alloy ingot partially grown and quenched on the ground can be back-melted and regrown in space under nearly steady state growth conditions. An identical "groundtruth" experiment was performed following the mission and a comparison between the properties of the crystals is described. The results indicate the importance of residual microgravity acceleration (approx. less than 0.4 mg) even in the sub-microgravity range for the slow solidification velocities and large density gradients.

Su, Ching-Hua↗
NASA NTRS1990

Influence of residual gravity on crystal growth processes

The effects of steady and time-dependent residual accelerations on representative melt and solution crystal growth systems have been investigated using numerical models. For the melt growth system, it was found that the lateral nonuniformity in crystal composition, depending on the particular operating conditions, can be very sensitive to the orientation of the steady component of the residual gravity vector down to 10 to the -6th g. Oscillatory residual accelerations (g-jitter) were found to lead to transients in the dopant distribution. For the solution growth, longtime simulations showed that at 10 to the -5th g, and the cooling rates used in Spacelab 3 experiments, diffusive transport dominates only in the beginning. Convective transport becomes increasingly significant after 3 to 5 hours, depending on the orientation of the crystal in the residual gravity field.

Rosenberger, F.↗
NASA NTRS1996

Control of crystal growth in water purification by directional freeze crystallization

A Directional Freeze Crystallization system employs an indirect contact heat exchanger to freeze a fraction of liquid to be purified. The unfrozen fraction is drained away and the purified frozen fraction is melted. The heat exchanger must be designed in accordance with a Growth Habit Index to achieve efficient separation of contaminants. If gases are dissolved in the liquid, the system must be pressurized.

Conlon, William M.↗
DOE OSTI2024

Single-crystal growth and characterization of antiferromagnetically ordered EuIn 2

Here, we report the single crystal growth and characterization of EuIn 2 , a magnetic topological semimetal candidate according to our density functional theory (DFT) calculations. We present results from electrical resistance, magnetization, Mössbauer spectroscopy, and X-ray resonant magnetic scattering (XRMS) measurements. We observe three magnetic transitions at T N1 ~ 14.2 K, T N2 ~ 12.8 K and T N3 ~ 11 K, signatures of which are consistently seen in anisotropic temperature dependent magnetic susceptibility and electrical resistance data. Mössbauer spectroscopy measurements on ground crystals suggest an incommensurate sinusoidally modulated magnetic structure below the transition at T N1 ~ 14 K, followed by the appearance of higher harmonics in the modulation on further cooling roughly below T N2 ~ 13 K, before the moment distribution squaring up below the lowest transition around T N3 ~ 11 K. XRMS measurements showed the appearance of magnetic Bragg peaks below T N1 ~ 14 K, with a propagation vector of $τ$ = ($τ_h$, $\overline{τ}_h$, 0), with $τ_h$ varying with temperature, and showing a jump at T N3 ~ 11 K. The temperature dependence of $τ_h$ between ~ 11 K and 14 K shows incommensurate values consistent with the Mössbauer data. XRMS data indicate that $τ_h$ remains incommensurate at low temperatures and locks into $τ_h$ = 0.3443(1).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1983

Barrier for Continuous-Crystal-Growth Crucible

Properly designed openings permit free flow of melt while restraining pellets. Redesigned partition between growth region and melt-replenishment region of crystal-growth crucible makes it less likely crucible will run out of feed material in middle of cycle. Supply of molten silicon is maintained by addition of silicon pellets to compartment at one end of heated crucible, and partition or barrier is required to hold pellets while allowing melted silicon to flow from compartment.

Skutch, M. E.↗
NASA NTRS1988

Temperature Fluctuations During Crystal Growth

Technique developed to deconvolve period and relative amplitude of fluctuations of heat flow inBridgman crystal growth. Temperature-measuring device with enough sensitivity and frequency response to make desired measurements inserted close as possible to substance monitored. Time-dependent temperature response recorded, and time domain response converted to frequency domain for further analysis. Fast fourier transform (FFT) of data on temperature oscillations shows particular behavior at some specific frequencies corresponding with striations, or defects observed on crystal. Useful procedure to help determine sources of some growth-induced crystalline defects. Other processes sensitive to small temperature fluctuations, such as diffusion, precipitation, and corrsion, benefit from technique.

Fripp, Archibald L., Jr.↗
NASA NTRS1992

Laser scattering in a hanging drop vapor diffusion apparatus for protein crystal growth in a microgravity environment

One type of hardware used to grow protein crystals in the microgravity environment aboard the U.S. Space Shuttle is a hanging drop vapor diffusion apparatus (HDVDA). In order to optimize crystal growth conditions, dynamic control of the HDVDA is desirable. A critical component in the dynamically controlled system is a detector for protein nucleation. We have constructed a laser scattering detector for the HDVDA capable of detecting the nucleation stage. The detector was successfully tested for several scatterers differing in size using dynamic light scattering techniques. In addition, the ability to detect protein nucleation using the HDVDA was demonstrated for lysozyme.

Casay, G. A.↗
NASA NTRS1998

Bulk Crystal Growth of Nonlinear Optical Organic Materials Using Inverted Vertical Gradient Freeze Method

A new process for producing large bulk single crystals of benzil (C6H5COCOC6H5) is reported in this paper. Good quality crystals have been successfully grown using this approach to crystal growth. This method seems to be very promising for other thermally stable NLO organic materials also. The entire contents vycor crucible 1.5 inch in diameter and 2 inch deep was converted to single crystal. Purity of the starting growth material is also an important factor in the final quality of the grown crystals. The entire crystal can be very easily taken out of the crucible by simple maneuvering. Initial characterization of the grown crystals indicated that the crystals are as good as other crystals grown by conventional Bridgman Stockbarger technique.

Choi, J.↗