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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 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
NASA NTRS1977

Web-dendritic growth

The effects of various machine design parameters on the growth of web dendritic silicon ribbon were investigated. Ribbons were grown up to lengths of one meter, with widths increasing linearly up to one cm at the point of termination of growth. Thermal data were collected and evaluated for actual seeding and growth with variations in parameters affecting heat loss. It was found that for suitable growth, the mechanical system should be very rigid and stable, and the tolerances and specifications of the quartz crucibles must be far tighter than normal quartz tolerances. The widening rates of the ribbons were found to be a function of the temperature gradient rather than the temperature differences alone. A twin spacing in the seed of 3 microns to 2 microns was found to be unfavorable for growth; whereas spacing of 0.9 microns to 2 microns and 8 microns to 2 microns were favorable. Thermal modeling studies of the effects of furnace design parameters on the temperature distributions in melt and the growth of the dendritic web ribbon showed that the pull rate of the ribbon is strongly dependent on the temperature of the top thermal shield, the spacing between this shield and the melt, and the thickness of the growing web.

Hilborn, R. B.↗
NASA NTRS1999

Effects of Melt Processing on Evolution of Structure in PEEK

We report on the effects of melt processing temperature on structure formation in Poly(ether-ether-ketone), PEEK. Real time Small Angle X-ray Scattering, SAXS, and thermal analysis are used to follow the melting behavior after various stages of processing. Assignment of peaks to structural entities within the material, the relative perfection of the crystals, and the possibility of their reorganization, are all influenced by the melt processing history. With the advent of high intensity synchrotron sources of X-radiation, polymer scientists gain a research tool which, when used along with thermal analysis, provides additional structural information about the crystals during growth and subsequent melting. PEEK is an engineering thermoplastic polymer with a very high glass transition temperature (145 C) and crystal melting point (337 C). PEEK has been the subject of recent studies by X-ray scattering in which melt and cold crystallization were followed in real-time. X-ray scattering and thermal studies have been used to address the formation of dual endothermic response which has been variously ascribed to lamellar insertion, dual crystal populations, or melting followed by re-crystallization. Another important issue is whether all of the amorphous phase is located in interlamellar regions, or alternatively whether some is located in "pockets" away from the crystalline lamellar stacks. The interpretation of scattering from lamellar stacks varies depending upon whether such amorphous pockets are formed. Some groups believe all of the amorphous phase is interlamellar. This leads to selection of a smaller thickness for the crystals. Other groups suggest that most amorphous phase is not interlamellar, and this leads to the suggestion that the crystal thickness is larger than the amorphous layer within the stacks. To investigate these ideas, we used SAXS and Differential Scanning Calorimetry to compare results of single and dual stage melt crystallization of PEEK using a treatment scheme involving annealing/crystallization at T(sub a1) followed by annealing at T(sub a2) where either T(sub a1) < T(sub a2) or T(sub a1) > T(sub a2). We proposed a model to explain multiple melting endotherms in PPS, treated according to one or two-stage melt or cold crystallization. Key features of this model are that multiple endotherms: (1) are due to reorganization/recrystallization after cold crystallization; and, (2) are dominated by crystal morphology after melt crystallization at high T. In other words, multiple distinct crystal populations are formed by the latter treatment, leading to observation of multiple melting. PEEK 45OG pellets (ICI Americas) were the starting material for this study. Films were compression molded at 400 C, then quenched to ice water. Samples were heated to 375 C in a Mettler FP80 hot stage and held for three min. to erase crystal seeds before cooling them to T(sub a1) = 280 C . Samples were held at T(sub a2) for a period of time, then immediately heated to 360 C. In the second treatment samples were held at T(sub a1) = 31 C for different crystallization times t(sub c) then cooled to 295 C and held 15 min. In situ (SAXS) experiments were performed at the Brookhaven National Synchrotron Light Source with the sample located inside the Mettler hot stage. The system was equipped with a two-dimensional position sensitive detector. The sample to detector distance was 172.7 cm and the X-ray wavelength was 1.54 Angstroms. SAXS data were taken continuously during the isothermal periods and during the heating to 360 C at 5 C/min. Each SAXS scan was collected for 30 sec. Since the samples were isotropic, circular integration was used to increase the signal to noise ratio. After dual stage melt crystallization with T(sub a1) < T(sub a2) the lower melting endotherm arises from holding at T(sub a1). During cooling a broad distribution of crystals forms, and the low-melting tail is perfected during T(sub al). Heating to T(sub a2) melts these imperfect crystals and allows others with greater average long spacing to form in their place. After dual stage crystallization with T(sub a1) > T(sub a2), the amount of space remaining for additional growth at T(sub a2) depends upon the holding time at T(sub a1). The long period of crystals formed at T(sub a2) is smaller than that formed at T(sub a1) due to growth in a now-restricted geometry. Perfection of crystals is seen as an increase of the intensity of the population scattering at higher s, while the intensity of the population scattering at lower s stays constant. During heating from below to above the minor endotherm, we see rapid decrease of the intensity of the X-ray scattering corresponding to the population of crystals scattering in the shoulder. Another important observation is that after the sample is annealed at 295 C, the shoulder intensity is restored once again. The population scattering at higher s remains longer before it disappears in the sample treated to the second stage of melt crystallization, compared to the sample crystallized with a single stage. This could be interpreted as an effect of continued perfection of the less perfect population, which is also reflected in the increased melting temperature of the smaller endotherm as the holding time at 295 C increases. In the corresponding DSC scans we see a shift in the area and the peak temperature of the lower melting endotherm with an increase of the annealing time.

Georgiev, Georgi↗
NASA NTRS1999

Determination of the Wetting Angle of Germanium and Germanium-Silicon Melts on Different Substrate Materials

During Bridgman growth of semiconductors detachment of the crystal and the melt meniscus has occasionally been observed, mainly under microgravity (microg) conditions. An important factor for detached growth is the wetting angle of the melt with the crucible material. High contact angles are more likely to result in detachment of the growing crystal from the ampoule wall. In order to achieve detached growth of germanium (Ge) and germanium-silicon (GeSi) crystals under 1g and microg conditions, sessile drop measurements were performed to determine the most suitable ampoule material as well as temperature dependence of the surface tension for GeSi. Sapphire, fused quartz, glassy carbon, graphite, SiC, pyrolytic Boron Nitride (pBN), AIN, and diamond were used as substrates. Furthermore, different cleaning procedures and surface treatments (etching, sandblasting, etc.) of the same substrate material and their effect on the wetting behavior were studied during these experiments. pBN and AIN substrates exhibited the highest contact angles with values around 170 deg.

Kaiser, Natalie↗
NASA NTRS1998

Melt Convection Effects in the Bridgman Crystal Growth of an Alloy Under Microgravity Conditions

The solidification of a dilute bismuth-tin alloy under Bridgman crystal growth conditions is investigated in support of NASA's MEPHISTO space shuttle flight experiment. Computations are performed in two-dimensions with a uniform grid. The simulation includes the species-concentration, temperature and flow fields, as well as conduction in the ampoule. Fully transient simulations have been performed; no simplifying steady state approximations are used. Results are obtained under microgravity conditions for pure bismuth, and Bismuth-0.1 at.% Sn and Bi-1.0 at.% Sn alloys. The concentration dependence of the melting temperature is neglected; the solid/liquid interface temperature is assumed to be the melting temperature of pure bismuth for all cases studied. For the Bi-1.0 at.% Sn case the results indicate that a secondary convective cell, driven by solutal gradients, forms near the interface. The magnitude of the velocities in this cell increases with time; this causes increasing solute segregation at the liquid/solid interface.

Simpson James E.↗
NASA NTRS1974

Analytics of crystal growth in space

Two crystal growth processes considered for spacelab experiments were studied to anticipate and understand phenomena not ordinarily encountered on earth. Computer calculations were performed on transport processes in floating zone melting and on growth of a crystal from solution in a spacecraft environment. Experiments intended to simulate solution growth at micro accelerations were performed.

Wilcox, W. R.↗
NASA NTRS2003

Studies of Nucleation and Growth, Specific Heat and Viscosity of Undercooled Melts of Quasicrystal and Polytetrahedral-Phase Forming Alloys

From extensive ground based work on the phase diagram and undercooling studies of Ti-Zr-Ni alloys, have clearly identified the composition of three different phases with progressively increasing polytetrahedral order such as, (Ti/Zr), the C14 Laves phase, and the i-phase, that nucleate directly from the undercooled liquid. The reduced undercooling decreases progressively with increasing polytetrahedral order in the solid, supporting Frank s hypothesis. A new facility for direct measurements of the structures and phase transitions in undercooled liquids (BESL) was developed and has provided direct proof of the primary nucleation of a metastable icosahedral phase in some Ti-Zr-Ni alloys. The first measurements of specific heat and viscosity in the undercooled liquid of this alloy system have been completed. Other than the importance of thermo-physical properties for modeling nucleation and growth processes in these materials, these studies have also revealed some interesting new results (such as a maximum of C(sup q, sub p) in the undercooled state). These ground-based results have clearly established the necessary background and the need for conducting benchmark nucleation experiments at the ISS on this alloy system.

Kelton, K. F.↗
NASA NTRS2016

Growth Mechanism of Nanowires: Ternary Chalcogenides

In the past two decades there has been a large rise in the investment and expectations for nanotechnology use. Almost every area of research has projected improvements in sensors, or even a promise for the emergence of some novel device technologies. For these applications major focuses of research are in the areas of nanoparticles and graphene. Although there are some near term applications with nanowires in photodetectors and other low light detectors, there are few papers on the growth mechanism and fabrication of nanowire-based devices. Semiconductor nanowires exhibit very favorable and promising optical properties, including high transparency and a several order of magnitude better photocurrent than thin film and bulk materials. We present here an overview of the mechanism of nanowire growth from the melt, and some preliminary results for the thallium arsenic selenide material system. Thallium arsenic selenide (TAS) is a multifunctional material combining excellent acousto-optical, nonlinear and radiation detection properties. We observed that small units of (TAS) nanocubes arrange and rearrange at moderate melt undercooling to form the building block of a nanowire. In some cases very long wires (less than mm) are formed. Since we avoided the catalyst, we observed self-nucleation and uncontrolled growth of wires from different places.

Singh, N. B.↗
NASA NTRS1974

Containerless processing of single crystals in low-G environment

Experiments on containerless crystal growth from the melt were conducted during Skylab missions SL3 and SL4 (Skylab Experiment M-560). Six samples of InSb were processed, one of them heavily doped with selenium. The concept of the experiment is discussed and related to general crystal growth methods and their merits as techniques for containerless processing in space. The morphology of the crystals obtained is explained in terms of volume changes associated with solidification and wetting conditions during solidification. All samples exhibit extremely well developed growth facets. Analysis by X-ray topographical methods and chemical etching shows that the crystals are of high structural perfection. Average dislocation density as revealed by etching is of the order of 100 per sq cm; no dislocation clusters could be observed in the space-grown samples. A sequence of striations that is observed in the first half of the selenium-doped sample is explained as being caused by periodic surface breakdown.

Walter, H. U.↗
DOE OSTI2022

Comprehensive view of microscopic interactions between DNA-coated colloids

Abstract The self-assembly of DNA-coated colloids into highly-ordered structures offers great promise for advanced optical materials. However, control of disorder, defects, melting, and crystal growth is hindered by the lack of a microscopic understanding of DNA-mediated colloidal interactions. Here we use total internal reflection microscopy to measure in situ the interaction potential between DNA-coated colloids with nanometer resolution and the macroscopic melting behavior. The range and strength of the interaction are measured and linked to key material design parameters, including DNA sequence, polymer length, grafting density, and complementary fraction. We present a first-principles model that screens and combines existing theories into one coherent framework and quantitatively reproduces our experimental data without fitting parameters over a wide range of DNA ligand designs. Our theory identifies a subtle competition between DNA binding and steric repulsion and accurately predicts adhesion and melting at a molecular level. Combining experimental and theoretical results, our work provides a quantitative and predictive approach for guiding material design with DNA-nanotechnology and can be further extended to a diversity of colloidal and biological systems.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
NASA NTRS2001

Studies of Nucleation, Growth, Specific Heat, and Viscosity of Undercooled Melts of Quasicrystals and Polytetrahedral-Phase-Forming Alloys

Undercooling experiments and thermal physical property measurements of metallic alloys on the International Space Station (ISS) are planned. This recently-funded research focuses on fundamental issues of the formation and structure of highly-ordered non-crystallographic phases (quasicrystals) and related crystal phases (crystal approximants), and the connections between the atomic structures of these phases and those of liquids and glasses. It extends studies made previously by us of the composition dependence of crystal nucleation processes in silicate and metallic glasses, to the case of nucleation from the liquid phase. Motivating results from rf-levitation and drop-tube measurements of the undercooling of Ti/Zr-based liquids that form quasicrystals and crystal approximants are discussed. Preliminary measurements by electrostatic levitation (ESL) are presented.

Kelton, K. F.↗
NASA NTRS2002

Studies of Nucleation and Growth, Specific Heat and Viscosity of Undercooled Melts of Quasicrystals and Polytetrahedral-Phase-Forming Alloys

The local atomic structures of undercooled liquid metals are presumed to be icosahedral; this order is incompatible with translational periodicity, constituting a barrier to the nucleation of the crystal phase. The extended atomic structure of the icosahedral quasicrystal (i-phase) is similar to that presumed in the undercooled liquid. Therefore, a comparison of the maximum undercooling in alloys that form the i-phase with those that form crystal phases provides a probe of the liquid structure.

Kelton, K. F.↗
NASA NTRS2003

Studies of Nucleation and Growth, Specific Heat and Viscosity of Undercooled Melts of Quasicrystals and Polytetrehedral-Phase-Forming Alloys

By investigating the properties of quasicrystals and quasicrystal-forming liquid alloys, we may determine the role of ordering of the liquid phase in the formation of quasicrystals, leading to a better fundamental understanding of both the quasicrystal and the liquid. A quasicrystal is solid characterized by a symmetric but non-periodic arrangement of atoms, usually in the form of an icosahedron (12 atoms, 20 triangular faces). It is theorized that the short-range order in liquids takes this same form. The degree of ordering depends on the temperature of the liquid, and affects many of the liquid s properties, including specific heat, viscosity, and electrical resistivity. The MSFC role in this project includes solidification studies, phase diagram determination, and thermophysical property measurements on the liquid quasicrystal-forming alloys, all by electrostatic levitation (ESL). The viscosity of liquid quasicrystal-forming alloys is measured by the oscillating drop method, both in the stable and undercooled liquid state. The specific heat of solid, undercooled liquid, and stable liquid are measured by the radiative cooling rate of the droplets.

Source record↗
DOE OSTI2020

Method for achieving sustained anisotropic crystal growth on the surface of a silicon melt

An apparatus for growing a crystalline sheet from a melt includes a cold block assembly. The cold block assembly may include a cold block and a shield surrounding the cold block and being at an elevated temperature with respect to that of the cold block, the shield defining an opening disposed along a surface of the cold block proximate a melt surface that defines a cold area comprising a width along a first direction of the cold block, the cold area operable to provide localized cooling of a region of the melt surface proximate the cold block. The apparatus may further include a crystal puller arranged to draw a crystalline seed in a direction perpendicular to the first direction when the cold block assembly is disposed proximate the melt surface.

36 MATERIALS SCIENCE↗
NASA NTRS1982

Effect of heat transfer of melt/solid interface shape and solute segregation in Edge-Defined Film-Fed growth - Finite element analysis

The effects of the heat transfer environment in Edge-Defined Film-Fed Growth on melt-solid interface shape and lateral dopant segregation are studied by finite-element analysis of two-dimensional models for heat and mass transfer. Heat transfer configurations are studied that correspond to the uniform surroundings assumed in previous models and to lowand high-speed growth systems. The maximum growth rate for a silicon sheet is calculated and the range of validity of one-dimensional heat transfer models is established. The lateral segregation that results from curvature of the solidification interface is calculated for two solutes, boron and aluminum. In this way, heat transfer is linked directly to the uniformity of the product crystal.

Ettouney, H. M.↗
NASA NTRS1981

Development of advanced Czochralski growth process to produce low cost 150 kg silicon ingots from a single crucible for technology readiness

Six growth runs used the Kayex-Hameo Automatic Games Logic (AGILE) computer based system for growth from larger melts in the Mod CG2000. The implementation of the melt pyrometer sensor allowed for dip temperature monitoring and usage by the operator/AGILE system. Use of AGILE during recharge operations was successfully evaluated. The tendency of crystals to lose cylindrical shape (spiraling) continued to be a problem. The hygrometer was added to the Furnace Gas Analysis System and used on several growth runs. The gas chromatograph, including the integrator, was also used for more accurate carbon monoxide concentration measurements. Efforts continued for completing the automation of the total Gas Analysis System. An economic analysis, based on revised achievable straight growth rate, is presented.

Lane, R. L.↗
NASA NTRS1996

Convection during Thermally Unstable Solidification of Pb-Sn in a Magnetic Field

Convection and macrosegregation in directionally solidified hypoeutectic Pb-38 wt pct Sn and hypereutectic Pb-64.5 wt pct Sn have been examined during upward and downward growth. Temperature fluctuations are observed along the length of the melt column during downward growth. With increasing Rayleigh number, these fluctuations change from none, to cyclic, to time periodic having multiple harmonics, and finally to random. At the higher convective driving force of 350 K temperature inversion, the transverse magnetic field decreased convective levels, strong random temperature fluctuations (flows) becoming smaller and periodic. The maximum field of 0.45 T was unable to completely eliminate convection. For the lower convective driving force of 150 K temperature inversion, the 0.05 T magnetic field decreased flows, and at 0.15 T, the field caused a dramatic decrease in the characteristic frequency of the temperature fluctuations, indicating a change in the nature of the flow, the waveform of the temperature fluctuations changing from sinusoidal to a pulsed wave. Temperature fluctuations and time delays between thermocouples were used to estimate flow velocities. Irrespective of the convection in the bulk melt (ahead of the mushy zone), longitudinal macrosegregation occurs only if the interdendritic melt mixes with the bulk melt.

Song, H.↗
DOE OSTI2026

Which way does the dendrite grow? Competition among epitaxy, preferred growth direction, and thermal gradients in powder bed fusion additive manufacturing

The as-processed microstructure of metal alloy parts manufactured through laser powder bed fusion (LPBF) is heavily derived from the cellular dendritic solidification. The growth direction of dendrites within the melt pool is determined through competition among epitaxial growth, preferred growth directions, and maximum thermal gradients. However, the dominant factor and the specific role of each in developing melt pool microstructures remain unknown. Here, in this study, we performed single laser track scans on an SS316L single crystal substrate and combined experimental characterization of microstructure and crystal orientations with Computational Fluid Dynamics simulations of thermal gradients to evaluate the role of each factor in determining dendritic growth direction and evolution. Our results reveal that epitaxial growth dominates microstructure development by preferentially growing along a single 〈100〉 variant of the single crystal substrate adjacent to the melt pool boundary. Under LPBF’s highly curved and rapidly evolving thermal field, this preferential dendrite variant selection and its continued growth from the melt pool boundary to the centerline are governed by the local temperature gradient magnitude at the solid-liquid interface, rather than by the instantaneous maximum temperature gradient direction alone. Using these findings, we successfully predict changes in the dendrite growth direction with changing laser scan direction on a single crystal substrate, and show that the geometric melt pool centerline can deviate from the microstructural centerline because asymmetric local temperature gradient magnitudes transiently limit growth, resulting in different dendrite travel distances on each side of the melt pool.

36 MATERIALS SCIENCE↗
NASA NTRS2001

Characterization of Surface Features in Detached Grown GeSi Crystals

The growth of detached crystals by the Bridgman technique, in which the growing crystal is not in contact with the crucible wall, has been observed both on earth and in microgravity conditions. At present, the mechanisms contributing to the detachment are not completely understood and until recently detachment has not been reproducibly obtained. It is commonly understood that the main factors that promote the occurrence of detached growth include: high contact angle between the melt and the crucible material, high growth angle, and a pressure difference between the annular gap around the solid below the melt and the volume above the melt along the meniscus. These parameters were varied in Bridgman growth experiments to determine the conditions required to achieve detached growth terrestrially in Ge and GeSi alloys. These experiments are in preparation for experiments on the International Space Station (ISS). The detailed objectives of the flight experiments and a description of the growth methods employed are the subject of another presentation at this Congress. Detached crystals were achieved repeatedly in pyrolytic boron nitride ampoules when a pressure difference was employed. All crystals, except for those grown in fused silica ampoules, were easily removed from their containers; however, this fact alone is not sufficient to infer detached growth. Detachment was verified by comparing profilometer measurements of the radius of the samples with observations of the sample surfaces using optical and electron microscopy. The surfaces of the attached areas of the crystals had the same shape and surface texture as the interior crucible wall. Regions of detached growth contained many unique features and crystal facets could usually be observed. Several of these surface features have been correlated with mechanisms of detachment or free surface growth in general and others to processing events or conditions. These results will be compared with observations of surface features on detached regions of microgravity grown crystals.

Cobb, S. D.↗