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NASA NTRS2012

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Kim, Hyun Jung↗

NASA NTRS1994

Convection and morphological stability during directional solidification

For growth of a vicinal face at constant velocity, the effect of anisotropic interface kinetics on morphological stability is calculated for a binary alloy. The dependence of the interface kinetic coefficient on crystallographic orientation is based on the motion and density of steps. Anisotropic kinetics give rise to traveling waves along the crystal-melt interface, and can lead to a significant enhancement of morphological stability. The stability enhancement increases as the orientation approaches a singular orientation and as the solidification velocity increases. Shear flows interact with the traveling waves and, depending on the direction of the flow, may either stabilize or destabilize the interface. Specific calculations are carried out for germanium-silicon alloys.

Coriell, Sam R.↗

DOE OSTI2025

Interface Nucleus Templating of Modular Intermetallic Morphologies: Chemical Pressure Complementarity, Columnar Domains, and Complex Disorder in Y 13 Ag 42.7 Zn 29.7

One element of the diversity of intermetallic phases is the formation of complex structures from the assembly of fragments of simpler structures. Recently, we devised the Interface Nuclear Approach as a model for understanding such modular arrangements, in which the intergrowth of different structures is driven by chemical pressure (CP) relief at shared motifs at the domain interfaces, referred to as interface nuclei. In this Article, we present the synthesis, crystal structure, and CP analysis of a new compound that expands on this theme, Y 13 Ag 42.7 Zn 29.7 . Its hexagonal structure contains interpenetrating domains based on the CaPd 5+x and EuMg 5 types. The CaPd 5+x -based regions are reminiscent of the lamellar intergrowth structures previously observed in the Y−Ag−Zn system. In Y 13 Ag 42.7 Zn 29.7 , however, the domains have a different morphology, forming columns that adopt a hexagonal rod-packing. The geometrical features of the remaining spaces are assigned, using the program GrowDomain, to the cores of trigonal units of the EuMg 5 type, while layers of disordered atoms occur at heights along z where the parent structures are mismatched. At the CaPd 5+x -type/EuMg 5 -type interfaces, simple interface nucleus motifs with strong CP-complementarity can be identified, while their distribution within the parent structures supports the notion of templated architectures in modular intermetallics.

Chemical structure↗

NASA NTRS1990

Growth morphology with anisotropic surface kinetics

The morphological evolution of crystals growing from an incongruent vapor phase is studied using a Monte Carlo model, and the full range of growth morphologies is recovered. The diffusion in the bulk nutrient and the anisotropy in the interface kinetics are morphologically destabilizing and stabilizing, respectively. For a given set of simulation parameters and lattice symmetries there is a critical size, which scales linearly with the mean free path in the vapor, beyond which a crystal cannot retain its stable, macroscopically faceted growth shape. Surface diffusion stabilizes faceted growth on the shorter scale of the mean surface diffusion length. In simulations with a uniform drift superimposed on the random walk nutrient transport, crystal faces oriented toward the drift show enhanced morphological stability compared to the purely diffusive situation. Rotational drifts with periodic reversal of direction are morphologically stabilizing for all crystal facets.

Xiao, Rong-Fu↗

NASA NTRS1992

The kinematics of buoyancy induced mixing

A model problem to study mixing driven by buoyancy flow fields due to a time dependent body force which consists of a steady and an oscillatory component is considered. Flow fields generated by a time dependent body force, which consists of a steady and an oscillatory component from vibrations or g-jitter, mix two fluids inside a cavity by stretching and folding the interface into various morphological patterns. These patterns show two basic structures depending on the dominant components of the body force. These structures are whirls and tendrils, corresponding to the dominance of either the steady or oscillatory component, respectively. A combination of these structures also occurs in the interaction region. In this region the effect of the steady component opposes the oscillatory component and the result is to smooth the interface, and prevent breakup of the interface. For the parametric range considered, two basic flow regimes occur: convective and chaotic. In the convective regime, the morphological patterns are topological. In the chaotic regime, mixing occurs by a repetitive sequence of bubble formation, necking, and breakup which spreads the concentration field throughout the cavity. The length stretch of the interface increases exponentially with time. The dynamical system characteristics show that in the convective regime, at a point in space, the flow field is oscillatory with elliptical phase space trajectories, and its power spectrum indicates that the flow field responds to the corresponding input frequency. Whereas, in the chaotic regime, the flow field is aperiodic, the phase space trajectories show irregular patterns, and the power spectrum shows a broadband distribution.

Duval, Walter M. B.↗

NASA NTRS1980

SPAR VI Technical Report for Experiment 76-22: Directional Solidification of Magnetic Composites

Samples of eutectic Bi/MnBi were directionally solidified during a low-g interval aboard the SPAR 6 flight and in a l-g environment under identical furnace velocity and thermal conditions. The Bi/MnBi eutectic is characterized by a regular rod eutectic whose morphology may be sensitive to thermo-solutal convection and by its components, MnBi, which is ferromagnetic. Morphological analyses on samples show statistically smaller interrod spacings and rod diameters with respect to samples grown under identical solidification furnace conditions in l-g. An adjustment between the interrod spacing, growth velocity, and total undercooling at the solidification interface is proposed. Morphological analyses on samples grown in l-g indicate little difference between results for different growth orientations with respect to the gravity vector. The magnetic properties are significantly affected, however, by the presence of a nonequilibrium magnetic phase and the nonequilibrium phase transforms to the equilibrium ferromagnetic phase during isothermal heat treatment.

Pirich, R. G.↗

DOE OSTI2024

Heterogeneous Solid Electrolyte Interphase Interactions Dictate Interface Instability in Sodium Metal Electrodes

Sodium (Na) metal batteries have attracted recent attention due to their low cost and high abundance of Na. However, the advancement of Na metal batteries is impeded due to key challenges such as dendrite growth, solid electrolyte interphase (SEI) fracture, and low Coulombic efficiency. This study examines the coupled electro‐chemo‐mechanical interactions governing the electrodeposition stability and morphological evolution at the Na/electrolyte interface. The SEI heterogeneities influence transport and reaction kinetics leading to the formation of current and stress hotspots during Na plating. Further, it is demonstrated that the heterogeneity‐induced Na metal evolution and its influence on the stress distribution critically affect the mechanical overpotential, contributing to a faster SEI failure. The analysis reveals three distinct failure mechanisms—mechanical, transport, and kinetic—that govern the onset of instabilities at the interface. Finally, a comprehensive comparative study of SEI failure in Na and lithium (Li) metal anodes illustrates that the electrochemical and mechanical characteristics of the SEI are crucial in tailoring the anode morphology and interface stability. This work delineates mechanistic stability regimes cognizant of the SEI attributes and underlying failure modes and offers important guidelines for the design of artificial SEI layers for stable Na metal electrodes.

25 ENERGY STORAGE↗

NASA NTRS1985

Crystal Growth Research in Space

The objectives of this work are to develop growth techniques and theory leading to improved bulk growth of semiconductor single crystals. Ground based experiments will be complemented by experiments carried out in the low-g environment provided by the space shuttle. Analytical studies and laboratory investigations are being conducted to better define the causes of crystalline defects and inhomogeneities. The compound semiconductor lead-tin-telluride is being used as the modeling material. Theoretical techniques are being developed to predict the thermal and solutal fields which are present during bulk growth from a melt. Techniques for measuring the thermophysical properties of semiconductors at high temperatures have been developed. During the past year electrochemical etching techniques have been developed for delineation of inhomogeneous regions in crystals. Thermal diffusivity measurements have been completed for the solid and liquid phases of PbTe and PbSnTe. Preliminary results have been obtained on the effects on crystal morphology of gravity, interface shape and interaction between the melt and the container.

Crouch, R. K.↗

NASA NTRS2003

Advanced Technology Development: Solid-Liquid Interface Characterization Hardware

Characterizing the solid-liquid interface during directional solidification is key to understanding and improving material properties. The goal of this Advanced Technology Development (ATD) has been to develop hardware, which will enable real-time characterization of practical materials, such as aluminum (Al) alloys, to unprecedented levels. Required measurements include furnace and sample temperature gradients, undercooling at the growing interface, interface shape, or morphology, and furnace translation and sample growth rates (related). These and other parameters are correlated with each other and time. A major challenge was to design and develop all of the necessary hardware to measure the characteristics, nearly simultaneously, in a smaller integral furnace compatible with existing X-ray Transmission Microscopes, XTMs. Most of the desired goals have been accomplished through three generations of Seebeck furnace brassboards, several varieties of film thermocouple arrays, heaters, thermal modeling of the furnaces, and data acquisition and control (DAC) software. Presentations and publications have resulted from these activities, and proposals to use this hardware for further materials studies have been submitted as sequels to this last year of the ATD.

Source record↗

NASA NTRS1984

Morphological stability in the presence of fluid flow in the melt

Recent experiments have shown that the presence of a vertical buoyancy-driven flow adjacent to an initially cylindrical crystal-melt interface may produce a time-dependent helical deformation of the interface, with a rotation period ranging from several minutes to many hours, depending upon the width of the melt. The temperature distribution is such that the interface is expected to be morphologically stable in the absence of fluid flow. A linear stability analysis reveals that the instability is due to a coupling between a basic hydrodynamic instability in the buoyant flow and the deformable boundary separating the two phases. The crystal-melt interface lowers the critical Grashof number of an analogous rigid-walled system by an order of magnitude for succinonitrile with a Prandtl number P = 22.8; furthermore, the hydrodynamic mode that is actually destabilized by the interface is not the least stable mode in the rigid-walled system for P = 22.8. The results show that the instability may be regarded either as a rather large alteration of a basic hydrodynamic instability by the crystal-melt interface, or as a significant modification of the morphological stability of the interface by the presence of the buoyant flow.

Mcfadden, G. B.↗

DOE OSTI2025

Investigation of Oxidation Mechanisms in HfS 2 and ZrS 2 via In Situ Electron Microscopy

Transition metal dichalcogenides (TMD) combine semiconducting properties with stability and are therefore widely studied for future microelectronic devices. However, applications require integration with a suitable dielectric at a planar, defect-free interface. For Hf- and Zr-based TMDs, the good dielectric properties of hafnia and zirconia imply that direct oxidation is a promising strategy, provided that a high-quality interface and suitable oxide morphology can be formed. Here, in this study, we investigate HfS 2 and ZrS 2 oxidation, aiming to understand pathways toward planar oxide layer formation and the mechanisms that determine the characteristics of the semiconductor/dielectric interface. We use conventional and environmental transmission electron microscopy to reveal changes in morphology and composition of the TMDs under different gaseous environments. We show that oxidation at ambient conditions causes compositional heterogeneities, with local replacement of S by O in both materials. Thermal oxidation causes desulfurization and formation of a smooth but defective oxide layer. In contrast, plasma oxidation appears the best-suited to forming a controlled TMD/dielectric interface with a smooth oxide layer and without major defects. These results provide insight into the opportunities available from HfS 2 and ZrS 2 through oxidation and suggest a materials processing strategy for electronic device fabrication.

HfS2↗

NASA NTRS1984

Thermoelectric and morphological effects of Peltier pulsing on directional solidification of eutectic Bi-Mn

Extensive in situ thermal measurements using Peltier Interface Demarcation (PID) during directional solidification of eutectic Bi/MnBi were carried out. Observations indicate that significant thermal transients occur throughout the sample as a result of the Peltier pulsing. The contributions of the Peltier, Thomson, and Joule heats were separated and studied as a function of pulse intensity and polarity. The Joule and the combined Peltier and Thomson thermal contributions were determined as a function of time during and after the current pulses, close to the solid/liquid interface. Variations of the Bi/MnBi particle morphology clearly reveal the interface shape, changes in interface velocity, meltback, and temporary loss of cooperative growth, as a result of the pulsing.

Silberstein, R. P.↗

NASA NTRS1987

Crystal growing from the melt

The mechanical and electrical properties of crystals produced by a unidirectional process depend strongly on the temperature and flow fields since these control the concentration of solute at the melt-crystal interface. The solute gradient there drives morphological instabilities that lead to cellular or dendritic interfaces. In the presentation several features of flow-solidification interactions will be discussed. These will include the effects of convection driven by density changes and buoyancy and the imposition of forced flow.

Davis, S. H.↗

DOE OSTI2025

Morphological Characterization of UO 2 F 2 and UF 4 Hydrolysis Products

Bulk samples of UO 2 F 2 and UF 4 were aged for 3 weeks under various relative humidity (RH) conditions to examine morphological changes associated with the hydrolysis of the materials. Aged samples were analyzed using scanning electron microscopy (SEM) to examine morphological changes, and Raman spectroscopy was used to correlate these changes with chemical composition. Little to no effect was evident for either material under lower RH conditions (i.e., 16% and 33%–38% RH). Under higher RH conditions (83% and 99%), multiple morphological changes were evident within the UO 2 F 2 samples because of the formation of hydrolysis products and possible interactions at the solid–vapor interface. Only one major morphological change was observed over the aging period—within the UF 4 system at 99% RH. This change can be attributed to the initial formation of anhydrous UO 2 F 2 and, subsequently, its hydrolysis products. After 37 weeks, UO 2 F 2 persisted as a hydrolysis product of UF4; however, no further hydrolysis products were observed. These results suggest that further research into a possible divergence of UF 4 and UO 2 F 2 degradation pathways is warranted.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1989

CdTe and ZnTe metal interface formation and Fermi-level pinning

Interfacial morphology and Fermi-level pinning behavior at the interfaces of Al, Ag, and Pt with UHV-cleaved CdTe and ZnTe are studied using X-ray photoelectron and ultraviolet photoemission spectroscopies. Results are compared to metal/HgCdTe interface formation. For Al/CdTe, a case is found where significantly greater intermixing occurs in CdTe than seen on HgCdTe. The Al/ZnTe interface is also more abrupt than Al/CdTe. Band bending results for interfaces of all three metals with p-CdTe and p-ZnTe are presented and implications for metal/HgZnTe interface formation are considered.

Wahi, A. K.↗

NASA NTRS1974

Apollo 17 orange glass - Textural and morphological characteristics of devitrification

Results of a study are presented concerning (1) the significance of nonexcentroradial growth textures in Apollo 17 orange glass and a comparison of these textures with those that develop in lunar and meteoritic chondrules, (2) the development and the nature of the crystalline-glass interface, and (3) the morphology and growth characteristics of olivine and of the opaque mineral oxides that result by devitrification of the orange glass. Observations of the orange glass soil are contrasted with subsequent partial melting of orange glass spherules that were incorporated into mildly metamorphosed breccias, and the quench textures that result in these larger cooling units are compared with the textures produced by supercooling of small particulate spherules. Results show that the expected changes in viscosity due to partial melting and recrystallization do not affect the shape of individual particles, and that neither the thermal gradients that need to be invoked across 20-100 micron spheres nor collision of glass particles during lava fountaining can account for the devitrification textures observed.

Haggerty, S. E.↗

DOE OSTI2026

Enabling Bipolar Membrane Manufacturing Using Microscopy

Bipolar membranes (BPMs) used for water treatment suffer from interface instabilities, causing premature failure and decreased performance. Recent research has highlighted the impacts of membrane morphology on mechanical behavior and performance. Improved material performance of thin film membranes requires enhanced transport properties coupled with better control of the mechanical characteristics to avoid premature failure of the film. Thus, morphology is a key parameter when developing and evaluating novel membrane materials. Microscopy offers unique advantages for nano-scale characterization of thin film membrane interfaces and morphologies. In this study, the interface junction of BPMs was evaluated using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX). BPMs were fabricated using (1) hot pressing lamination, (2) bench-scale solution casting, and (3) roll-to-roll sequential casting (R2R). Both commercial and in-house fabricated ion exchange membranes were used in the BPMs. The BPMs were comprised of a cation exchange membrane and an anion exchange membrane with a catalyst layer sandwiched in between. Cross sectional SEM and EDX images of the membrane interface junction were compared among the different fabrication techniques and materials. The bench cast catalyst layers were nonuniform compared to the R2R and hot pressed membranes, demonstrating the importance of precise catalyst application conditions. Different thicknesses of the BPMs and individual membrane layers revealed that polymer solution concentration needs to be optimized during manufacturing. This work shows that microscopy can identify key processing parameters that affect BPM interface junction quality at the microscale to enable manufacturing of high performance BPMs.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Enabling Roll-to-Roll Manufacturing of Bipolar Membranes Using Microscopy

36 MATERIALS SCIENCE↗