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Materials analysis by ultrasonics: Metals, ceramics, composites

Research results in analytical ultrasonics for characterizing structural materials from metals and ceramics to composites are presented. General topics covered by the conference included: status and advances in analytical ultrasonics for characterizing material microstructures and mechanical properties; status and prospects for ultrasonic measurements of microdamage, degradation, and underlying morphological factors; status and problems in precision measurements of frequency-dependent velocity and attenuation for materials analysis; procedures and requirements for automated, digital signal acquisition, processing, analysis, and interpretation; incentives for analytical ultrasonics in materials research and materials processing, testing, and inspection; and examples of progress in ultrasonics for interrelating microstructure, mechanical properties, and dynamic response.

Vary, Alex

Mixing Dynamics Induced by Traveling Magnetic Fields

Microstructural and compositional homogeneity in metals and alloys can only be achieved if the initial melt is homogeneous prior to the onset of solidification processing. Naturally induced convection may initially facilitate this requirement but upon the onset of solidification significant compositional variations generally arise leading to undesired segregation. Application of alternating magnetic fields to promote a uniform bulk liquid concentration during solidification processing has been suggested. To investigate such possibilities an initial study of using traveling magnetic fields (TMF) to promote melt homogenization is reported in this work. Theoretically, the effect of TMF-induced convection on mixing phenomena is studied in the laminar regime of flow. Experimentally, with and without applied fields, both: mixing dynamics by optically monitoring the spreading of an initially localized dye in transparent fluids and, compositional variations in metal alloys have been investigated.

Grugel, Richard N.

Mixing Dynamics Induced by Traveling Magnetic Fields

Microstructural and compositional homogeneity in metals and alloys can only be achieved if the initial melt is homogeneous prior to the onset of solidification processing. Naturally induced convection may initially facilitate this requirement but upon the onset of solidification significant compositional variations generally arise leading to undesired segregation. Application of alternating magnetic fields to promote a uniform bulk liquid concentration during solidification processing has been suggested. To investigate such possibilities an initial study of using traveling magnetic fields (TMF) to promote melt homogenization is reported in this work. Theoretically, the effect of TMF-induced convection on mixing phenomena is studied in the laminar regime of flow. Experimentally, with and without applied fields, both 1) mixing dynamics by optically monitoring the spreading of an initially localized dye in transparent fluids and, 2) compositional variations in metal alloys have been investigated.

Grugel, Richard N.

Measurements of radiated elastic wave energy from dynamic tensile cracks

The role of fracture-velocity, microstructure, and fracture-energy barriers in elastic wave radiation during a dynamic fracture was investigated in experiments in which dynamic tensile cracks of two fracture cofigurations of double cantilever beam geometry were propagating in glass samples. The first, referred to as primary fracture, consisted of fractures of intact glass specimens; the second configuration, referred to as secondary fracture, consisted of a refracture of primary fracture specimens which were rebonded with an intermittent pattern of adhesive to produce variations in fracture surface energy along the crack path. For primary fracture cases, measurable elastic waves were generated in 31 percent of the 16 fracture events observed; the condition for radiation of measurable waves appears to be a local abrupt change in the fracture path direction, such as occurs when the fracture intersects a surface flaw. For secondary fractures, 100 percent of events showed measurable elastic waves; in these fractures, the ratio of radiated elastic wave energy in the measured component to fracture surface energy was 10 times greater than for primary fracture.

Boler, Frances M.

Role of back stress in the creep behavior of particle strengthened alloys

Recent developments in the interpolation of high-temperature steady-state creep results have introduced the concept that the stress dependence of the creep rate should be in terms of the effective stress referred to as the applied stress minus a back stress. This paper reports on back stresses taken from data on a gamma-prime-strengthened wrought nickel-base superalloy, an oxide dispersion-strengthened ODS nickel-base solid solution alloy, and an ODS nickel-base superalloy. The effect of air versus vacuum environments and the effect of dynamic changes in the strengthening microstructures on the magnitude of the back stress are assessed. The role of modulus normalization and the back stress correction in determining the true creep activation energy are examined. It is shown that the high values of the apparent stress exponent 'n' of the steady-state creep equation can be easily explained through a relationship between n, the true stress exponent of steady-state creep, and the stress which when subtracted from the applied stress results in the effective driving stress acting on the mobile dislocations during creep.

Purushothaman, S.

Influence of the Si3N4 microstructure on its R-curve and fatigue behavior

The R-curve and fatigue behavior of a silicon nitride with large, highly elongated grains were compared to those of a silicon nitride with smaller, more equiaxed grains. The former was found to have higher toughness and a slightly rising R-curve which enhanced fatigue resistance, while the latter had constant toughness with crack length. The R-curve was attributed to crack deflection and grain pull-out. The microstructure did not influence the dynamic fatigue properties of the two ceramics, as both had good resistance to dynamic fatigue. The cyclic fatigue resistance of the large-grained Si3N4, however, was surprisingly low.

Tikare, Veena

Multiscale Modeling for the Analysis for Grain-Scale Fracture Within Aluminum Microstructures

Multiscale modeling methods for the analysis of metallic microstructures are discussed. Both molecular dynamics and the finite element method are used to analyze crack propagation and stress distribution in a nanoscale aluminum bicrystal model subjected to hydrostatic loading. Quantitative similarity is observed between the results from the two very different analysis methods. A bilinear traction-displacement relationship that may be embedded into cohesive zone finite elements is extracted from the nanoscale molecular dynamics results.

Glaessgen, Edward H.

Finite Element Simulation of the Direct Energy Deposition using Comsol Multiphysics

Direct Energy Deposition (DED) is an emerging technology extensively employed in metal Additive Manufacturing (AM). Despite its widespread industrial application, mathematical modeling in this domain remains challenging. This complexity arises from the intricate nature of the modeling approach and the nonlinear behavior of material parameters across a broad temperature range. Consequently, experimentalists often resort to a trial-and-error method to achieve structures with desired properties. However, this approach can be time-consuming and may not always yield parts with the requisite characteristics, highlighting the necessity for mathematical modeling to enhance manufacturing success. This study focuses on thin-walled manufacturing with a single bead thickness, adjusting laser parameters to produce such structures. The laser cladding speed, typical for DED manufacturing, is considered to be on the order of centimeters per second. The various wall thicknesses and heights are explored to discern the general characteristics of walls manufactured via this DED approach. Our modeling approach diverges from the conventional DED modeling based on activation-deactivation of predefined mesh domains, commonly implemented in many finite element codes. Instead, a method is proposed that effectively models layer cladding and melt pool dynamics, enabling predictions of the microstructure in the resulting structures. The formation mechanisms of cellular, dendritic columnar, and stray (equiaxed) grains, which arise from the interplay between nucleation and growth from the surface is analyzed. The study also examines the feasibility of microstructure formation to demonstrate the various thermal characteristics inherent in wall manufacturing. Our results illustrate how different process parameters influence the temperature gradient and cooling rate of the molten pool, subsequently affecting the primary dendrite arm spacing (PDAS). This modeling technique allows for the investigation of diverse thermal conditions, facilitating the prediction of microstructure and residual stresses in the manufactured parts.

modeling

Microstructure Characterization and Stress Corrosion Evaluation of Autogenous and Hybrid Friction Stir Welded Al-Cu-Li 2195 Alloy

Friction stir welding process is being evaluated for application on the Al-Cu-Li 2195 Super-Light Weight External Tank of the Space Transportation System. In the present investigation Al-Cu-Li 2195 plates were joined by autogenous friction stir welding (FSW) and hybrid FSW (friction stir welding over existing variable polarity plasma arc weld). Optical microscopy and transmission electron microscopy (TEM) were utilized to characterize microstructures of the weldments processed by both welding methods. TEM observations of autogenous FSW coupons in the center section of the dynamically-recrystallized zone showed an equiaxed recrystallized microstructure with an average grain size of approx. 3.8 microns. No T(sub 1), precipitates were present in the above-mentioned zone. Instead, T(sub B) and alpha precipitates were found in this zone with a lower population. Alternate immersion, anodic polarization, constant load, and slow strain tests were carried out to evaluate the general corrosion and stress-corrosion properties of autogenous and hybrid FSW prepared coupons. The experimental results will be discussed.

Li, Zhixian

Dynamic oxidation behavior of TD-NiCr alloy with different surface pretreatments

Oxidation tests of TD-NiCr alloy with different surface pretreatments were conducted in a Mach-5 arc-jet at 1200 C and 0.002 lb/sec flowing air environment. The mechanisms responsible for the observed oxidation behavior are examined. The presence of atomic oxygen in the air stream plays a significant role in determining the oxidation characteristic of the alloy. The rate of Cr2O3 vaporization by formation of volatile CrO3 is greatly enhanced by the flowing conditions. The typical microstructure of oxides formed in the dynamic tests consists of an external layer of NiO with a porous mushroom-type morphology, an intermediate layer of NiO and Cr2O3 oxide mixture, and a continuous inner layer of Cr2O3 in contact with the Cr-depleted alloy substrate. Three basic processes underlying the formation of mushroom-type NiO are identified and discussed. The oxidation rate is determined by the rate of vaporization of NiO. Surface pretreatment has a significant effect on the oxidation behavior of the alloy in the early stage of oxidation, but becomes less important as exposure time increases. Mechanical polishing induces surface recrystallization, but promotes the concurrence of external growth of NiO and internal oxidation of the alloy in the dynamic atmosphere.

Young, C. T.

Thermal Stir Welding Development at Marshall Space Flight Center

Solid state welding processes have become the focus of welding process development at NASA's Marshall Space Flight Center. Unlike fusion weld processes such as tungsten inert gas (TIG), variable polarity plasma arc (VPPA), electron beam (EB), etc., solid state welding processes do not melt the material during welding. The resultant microstructure can be characterized as a dynamically recrystallized morphology much different than the casted, dentritic structure typical of fusion weld processes. The primary benefits of solid state processes over fusion weld processes include superior mechanic properties and the elimination of thermal distortion and residual stresses. These solid state processes attributes have profoundly influenced the direction of advanced welding research and development within the NASA agency. Thermal Stir Welding (TSW) is a new solid state welding process being developed at the Marshall Space Flight Center. Unlike friction stir welding, the heating, stirring and forging elements of the weld process can be decoupled for independent control. An induction coil induces energy into a workpiece to attain a desired plastic temperature. An independently controlled stir rod, captured within non-rotating containment plates, then stirs the plasticized material followed by forging plates/rollers that work the stirred weld joint. The independent control (decoupling) of heating, stirring and forging allows, theoretically, for the precision control of microstructure morphology. The TSW process is being used to evaluate the solid state joining of Haynes 230 for ARES J-2X applications. It is also being developed for 500-in (12.5 mm) thick commercially pure grade 2 titanium for navy applications. Other interests include Inconel 718 and stainless steel. This presentation will provide metallurgical and mechanical property data for these high melting temperature alloys.

Ding, Robert J.

Stress Distribution During Deformation of Polycrystalline Aluminum by Molecular-Dynamics and Finite-Element Modeling

In this paper, a multiscale modelling strategy is used to study the effect of grain-boundary sliding on stress localization in a polycrystalline microstructure with an uneven distribution of grain size. The development of the molecular dynamics (MD) analysis used to interrogate idealized grain microstructures with various types of grain boundaries and the multiscale modelling strategies for modelling large systems of grains is discussed. Both molecular-dynamics and finite-element (FE) simulations for idealized polycrystalline models of identical geometry are presented with the purpose of demonstrating the effectiveness of the adapted finite-element method using cohesive zone models to reproduce grain-boundary sliding and its effect on the stress distribution in a polycrystalline metal. The yield properties of the grain-boundary interface, used in the FE simulations, are extracted from a MD simulation on a bicrystal. The models allow for the study of the load transfer between adjacent grains of very different size through grain-boundary sliding during deformation. A large-scale FE simulation of 100 grains of a typical microstructure is then presented to reveal that the stress distribution due to grain-boundary sliding during uniform tensile strain can lead to stress localization of two to three times the background stress, thus suggesting a significant effect on the failure properties of the metal.

Yamakov, V.

Microstructure of the solar wind

In this review microstructure is understood to summarize the dynamical properties of the solar wind that enter the fluid equations, usually employed to describe the overall flow, only in one or the other averaged form. Thus, first a description of the kinetic picture of the solar wind is given; it mainly involves the structure of the particle distributions in velocity space and associated instabilities. Waves and discontinuities are discussed next. Two selected examples are mentioned where the effects of waves and discontinuities play a role. Specific physical properties of the interplanetary magnetic irregularity spectrum and its relevance for cosmic ray propagation are discussed at the end.

Voelk, H. J.

Supercooling effects in Cu-10 wt pct Co alloys solidified at different cooling rates

Electromagnetic levitation and electron beam surface melting were employed to study the effects of supercooling and cooling rate on the solidification of Cu-10 wt pct Co alloys. Two major effects were observed in the supercooled alloys: the nucleation of a metastable copper-rich phase which contains 13 wt pct to 20 wt pct Co in samples supercooled between 105 and 150 K and liquid phase separation which occurs in samples supercooled 150 K or more. The microstructure of the electron beam melted surfaces consisted of very fine spheres which were similar to those of the sample supercooled more than 150 K but with a refined microstructure. The results indicate that a dynamic bulk supercooling of 150 K may exist in the molten pool during the solidification of electron beam melted surfaces.

Munitz, A.

High temperature dynamic modulus and damping of aluminum and titanium matrix composites

Dynamic modulus and damping capacity property data were measured from 20 to over 500 C for unidirectional B/Al (1100), B/Al (6061), B/SiC/Al (6061), Al2O3/Al, SiC/Ti-6Al-4V, and SiC/Ti composites. The measurements were made under vacuum by the forced vibration of composite bars at free-free flexural resonance near 2000 Hz and at amplitudes below 0.000001. Whereas little variation was observed in the dynamic moduli of specimens with approximately the same fiber content (50 percent), the damping of B/Al composites was found at all temperatures to be significantly greater than the damping of the Al2O3/Al and SiC/Ti composites. For those few situations where slight deviations from theory were observed, the dynamic data were examined for information concerning microstructural changes induced by composite fabrication and thermal treatment. The 270 C damping peak observed in B/Al (6061) composites after heat treatment above 460 C appears to be the result of a change in the 6061 aluminum alloy microstructure induced by interaction with the boron fibers. The growth characteristics of the damping peak suggest its possible value for monitoring fiber strength degration caused by excess thermal treatment during B/Al (6061) fabrication and use.

Dicarlo, J. A.

Reactive Infiltration of Silicon Melt Through Microporous Amorphous Carbon Preforms

The kinetics of unidirectional capillary infiltration of silicon melt into microporous carbon preforms have been investigated as a function of the pore morphology and melt temperature. The infiltrated specimens showed alternating bands of dark and bright regions, which corresponded to the unreacted free carbon and free silicon regions, respectively. The decrease in the infiltration front velocity for increasing infiltration distances, is in qualitative agreement with the closed-form solution of capillarity driven fluid flow through constant cross section cylindrical pores. However, drastic changes in the thermal response and infiltration front morphologies were observed for minute differences in the preforms microstructure. This suggests the need for a dynamic percolation model that would account for the exothermic nature of the silicon-carbon chemical reaction and the associated pore closing phenomenon.

Sangsuwan, P.

In Situ Observation of Growth Dynamics in DECLIC Directional Solidification Insert Onboard ISS: DSI-R Flight Campaign

The study of solidification microstructure formation is of utmost importance for materials design and processing, as solid-liquid interface patterns largely govern mechanical and physical properties. Pattern selection occurs under dynamic conditions of growth in which the initial morphological instability evolves nonlinearly and undergoes a reorganization process. The dynamic and nonlinear nature of this instability renders in situ observation of the interface an invaluable tool to gain knowledge on the time-evolution of the interface pattern. Transparent organic analogs, which solidify like metallic alloys, allow direct visualization of interface dynamics. Extensive ground-based studies of both metallic and organic bulk samples have established the presence of significant convection during solidification processes that alters the formation of interfacial microstructures. A reduced-gravity environment is therefore mandatory for fluid flow elimination in bulk samples. In the framework of the CNES project MISOL3D (MIcrostrutures de SOLidification 3D) and the NASA projects DSIP (Dynamical Selection of 3D Interface Patterns), SPADES (SPAtiotemporal Evolution of three-dimensional DEndritic array Structures) and CAMUS (ComputAtional Studies of MicrostrUcture Formation During Alloy Solidification in Microgravity), we participated in the development of the Directional Solidification Insert (DSI) of the DEvice for the study of Critical Liquids and Crystallization (DECLIC). The DECLIC-DSI is dedicated to in situ and real-time characterization of solid-liquid interface patterns during directional solidification of transparent alloys in diffusive transport regime. Between April 2010 and March 2011, the first ISS campaign (DSI) explored the entire range of microstructures resulting in unprecedented observations. A second campaign (DSI-R), performed between October 2017 and December 2018, in which the insert contained an alloy of higher solute concentration, allowed to complete the benchmark database. The increase of solute concentration resulted in well-developed dendritic patterns at lower velocities (lower interface curvature and larger tip radius). The microstructure resulting from dendritic growth is dominant in metallurgy so that it is fundamental to understand the mechanisms of its formation. The main aims of this experimental campaign are to understand: the mechanisms of the cell to dendrite transition, the fundamental mechanisms of sidebranching formation, the dependence of dendrite tip shapes on growth conditions, the interaction of primary array and secondary sidebranches, and the influence of subgrain boundaries on the spatiotemporal organization of the array structure. Preparation, analysis and interpretation of the experiments performed onboard ISS are considerably enhanced by experiments performed on ground using thin-samples (Pr. Trivedi’s group) and phase-field simulations of microstructure formation in a diffuse growth regime (Pr. Karma’s group). In this summary, we will present an initial assessment of the results obtained during the DSI-R campaign. Nomenclature Vp: pulling velocity G: thermal gradient L: solidified length rtip: tip curvature radius Acronyms/Abbreviations CADMOS: Centre d'Aide au Développement des activités en Micro-pesanteur et des Opérations Spatiales CNES: Centre National d’Études Spatiales DECLIC: Device for the study of Critical LIquids and Crystallization DSI: Directional Solidification Insert DSI-R: Directional Solidification Insert - Refurbish ISS: International Space Station NASA: National Aeronautics and Space Administration PF: phase-field SCN: Succinonitrile 3D: three-dimensional

Mota, F.L.

Simulating Space Weathering in the Transmission Electron Microscope via Dynamic in Situ Heating and Helium Irradiation of Olivine

The chemical composition, microstructure, and optical properties of grains on the surfaces of airless bodies are predominantly altered by micrometeorite impacts and solar wind irradiation. These processes drive space weathering and result in the formation of features including chemically-altered, amorphous grain rims, Fe nanoparticles (npFe), and vesiculated grain textures. These characteristics have been identified in returned samples from the surfaces of the Moon and asteroid Itokawa. In order to advance our understanding of the formation of these microstructural and chemical features in returned samples, we have simulated space weathering processes for a variety of materials via laboratory experiments. These experiments include ion irradiation to simulate solar wind exposure and laser irradiation and in situ heating to simulate micrometeorite impacts. While these experiments have provided considerable insight into the formation mechanisms of many space weathering features, they are predominantly static and typically performed separately. Here we present results from the simulated space weathering of olivine grains via He irradiation and dynamic heating, both performed in situ inside the transmission electron microscope (TEM). These experiments allow for the real-time observation of chemical and microstructural changes resulting from the superposed effects of ion irradiation and pulsed heating.

Thompson, M. S.