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DOE OSTI2021

Using Multigrain Crystallography to Explore the Microstructural Evolution of the α-Olivine to γ-Ringwoodite Transformation and ε-Mg2SiO4 at High Pressure and Temperature

The introduction of multigrain crystallography (MGC) applied in a laser-heated diamond anvil cell (LH-DAC) using synchrotron X-rays has provided a new path to investigate the microstructural evolution of materials at extreme conditions, allowing for simultaneous investigations of phase identification, strain state determination, and orientation relations across phase transitions in a single experiment. Here, we applied this method to a sample of San Carlos olivine beginning at ambient conditions and through the α-olivine → γ-ringwoodite phase transition. At ambient temperatures, by measuring the evolution of individual Bragg reflections, olivine shows profuse angular streaking consistent with the onset of yielding at a measured stress of ~1.5 GPa, considerably lower than previously reported, which may have implications for mantle evolution. Furthermore, γ-ringwoodite phase was found to nucleate as micron to sub-micron grains imbedded with small amounts of a secondary phase at 15 GPa and 1000 °C. Using MGC, we were able to extract and refine individual crystallites of the secondary unknown phase where it was found to have a structure consistent with the ε-phase previously described in chondritic meteorites.

36 MATERIALS SCIENCE↗

NASA NTRS1973

Investigation of solidification in zero-gravity environment: M553 sphere forming experiment. Nickel-silver alloy evaluation

The processing of nickel-silver alloy specimens in space is discussed. Four specimens were melted only partially, while a fifth was melted completely and assumed after solidification a perfectly spherical shape. Growth of the solid was epitaxial on the unmelted material or on the retaining sting and occurred without undercooling. Solidification was dendritic in all cases with nonequilibrium silver particles forming monotectically between dendrite arms. Substantial loss of silver by evaporation took place. Evaporation of the silver within internal gas cavities on the melt was followed by surface condensation after completion of solidification and cooling, leading to a silver-rich lining in these cavities. The material gave no microstructural evidence of any reduction in liquid convection.

Kattamis, T. Z.↗

NASA NTRS1977

Friction factor for isothermal and nonisothermal flow through porous media

Measurements were performed to determine the pressure drops for gaseous flow through porous materials of different microstructures, porosities, and thickness under isothermal and nonisothermal conditions at various temperature levels. Results were satisfactorily correlated by a simple equation relating the friction factor to the Reynolds number and porosities.

Koh, J. C.↗

NASA NTRS1982

Fundamentals of ultrasonic NDE for microstructure/material property interrelations

Some fundamental aspects of ultrasonic nondestructive evaluation for material properties and microstructure assessment are given. Ultrasonic wave interaction concepts, some recent findings, and practical ramifications are illustrated. The concepts are discussed in nonmathematical, narrative form. Additional information can be found in the references cited herein.

A. Vary↗

NASA NTRS1986

Making High-Porosity Alloy Spheroids

Noncontact process yields low-density, porous microstructure. Small spheroids of porous alloys with large surface area per unit volume produced by containerless processing method. Without container walls to serve as nucleation sites, alloy cools to well below normal freezing point without solidifying. Solidification then proceeds rapidly; interdendritic liquid pulled out by growing crystals, resulting in porous microstructure. The more rapid the cooling rate, the faster crystals grow and more porous solid becomes. Drop-tube method useful in creating porous microstructures from other materials including oxides, carbides, and organic materials. Other means of containerless processing - acoustic or air-jet levitation, low-gravity float melting, melt spinning, or jet spraying, adapted to process.

Ethridge, E. C.↗

NASA NTRS1986

Oxidation characteristics of 440 C CRES in gaseous oxygen (GOX) environments

The oxidation characteristics of 440 C corrosion-resistant steel are evaluated. The dependence of oxide color, type, and thickness, material hardness, and microstructure on temperature is examined. The effects of exposure time, passivation layer, and oxygen pressure on the oxide formation are investigated. A direct relationship between temperature and oxide color, formation, and thickness is detected. It is observed that the exposure time does not affect the microstructure or oxide color, type, or thickness; however, the passivation layer does affect oxide color and type.

Dennies, Daniel P.↗

NASA NTRS1989

A Monte Carlo-finite element model for strain energy controlled microstructural evolution - 'Rafting' in superalloys

This paper presents a specialized microstructural lattice model, MCFET (Monte Carlo finite element technique), which simulates microstructural evolution in materials in which strain energy has an important role in determining morphology. The model is capable of accounting for externally applied stress, surface tension, misfit, elastic inhomogeneity, elastic anisotropy, and arbitrary temperatures. The MCFET analysis was found to compare well with the results of analytical calculations of the equilibrium morphologies of isolated particles in an infinite matrix.

Gayda, J.↗

NASA NTRS1991

NASA-UVA Light Aerospace Alloy and Structures Technology Program (LA2ST)

The general objective of the Light Aerospace Alloy and Structures Technology (LA2ST) Program is to conduct interdisciplinary graduate student research on the performance of next generation, light weight aerospace alloys, composites, and associated thermal gradient structures in close collaboration with Langley researchers. Specific technical objectives are established for each research project. Relevant data and basic understanding of material behavior and microstructure, new monolithic and composite alloys, advanced processing methods, new solid and fluid mechanic analyses, measurement advances, and a pool of educated graduate students are sought.

Gangloff, Richard P.↗

NASA NTRS1993

Vaporization heat transfer of dielectric liquids on enhanced surfaces covered with screen wicks

Experiments were conducted to investigate the vaporization heat transfer characteristics for the dielectric liquid FC-72 on several wicking surfaces which may be used in flat-plate heat pipes. The wicking materials studied included microstructure enhanced surfaces and coarse surfaces covered with screen meshes. Experimental data for q versus deltaT curves and critical heat fluxes were obtained for the two different operating conditions of a heat pipe, evaporation, and shallow pool boiling. When the liquid level was above the heated surface, the height of the liquid level above the surface was varied from 0 to 10 mm. When the liquid level was below the heated surface, the distance from the liquid level to the edge of the surface was adjusted from 0 to 15 mm. Experimental results revealed that for shallow pool boiling when the heated surface was covered with a wire screen mesh, the heat transfer coefficient increased at lower heat fluxes but the critical heat flux (CHF) decreased for all the surfaces tested. In the case of evaporation, both CHF and the heat transfer coefficient increased as the microstructure surfaces were covered with screen meshes.

Gu, C. B.↗

NASA NTRS1993

Microstructural analysis of the 2195 aluminum-lithium alloy welds

The principal objective of this research was to explain a tendency of 2195 Al-Li alloy to crack at elevated temperature during welding. Therefore, a study was made on the effect of welding and thermal treatment on the microstructure of Al-Li Alloy 2195. The critical roles of precipitates, boundaries, phases, and other features of the microstructure were inferred from the crack propagation paths and the morphology of fracture surface of the alloy with different microstructures. Particular emphasis was placed on the microstructures generated by the welding process and the mechanisms of crack propagation in such structures. Variation of the welding parameters and thermal treatments were used to alter the micro/macro structures, and they were characterized by optical and scanning electron microscopy. A theoretical model is proposed to explain changes in the microstructure of welded material. This model proposes a chemical reaction in which gases from the air (i.e., nitrogen) release hydrogen inside the alloy. Such a reaction could generate large internal stresses capable to induce porosity and crack-like delamination in the material.

Talia, George E.↗

NASA NTRS1995

Low Cost Fabrication of Silicon Carbide Based Ceramics and Fiber Reinforced Composites

A low cost processing technique called reaction forming for the fabrication of near-net and complex shaped components of silicon carbide based ceramics and composites is presented. This process consists of the production of a microporous carbon preform and subsequent infiltration with liquid silicon or silicon-refractory metal alloys. The microporous preforms are made by the pyrolysis of a polymerized resin mixture with very good control of pore volume and pore size thereby yielding materials with tailorable microstructure and composition. Mechanical properties (elastic modulus, flexural strength, and fracture toughness) of reaction-formed silicon carbide ceramics are presented. This processing approach is suitable for various kinds of reinforcements such as whiskers, particulates, fibers (tows, weaves, and filaments), and 3-D architectures. This approach has also been used to fabricate continuous silicon carbide fiber reinforced ceramic composites (CFCC's) with silicon carbide based matrices. Strong and tough composites with tailorable matrix microstructure and composition have been obtained. Microstructure and thermomechanical properties of a silicon carbide (SCS-6) fiber reinforced reaction-formed silicon carbide matrix composites are discussed.

Singh, M.↗

NASA NTRS1992

Evaluation of microcrack thermal shock damage in ceramics: Modeling and experiment

In this paper we present an experimental and theoretical study of the effect of microcrack damage on ceramic properties. For the experimental investigation, ceramic samples of aluminum oxide and reaction bonded silicon nitride (RBSN) are used. Thermal shock treatment from different temperatures up to 1000 C is applied to produce the microcracks. Both surface and bulk ultrasonic wave methods are used to correlate the change of elastic constants to microstructural degradation and to determine the change in elastic anisotropy induced by microcrack damage. For the theoretical investigation, damage mechanics, which relates microstructural damage to material service life and mechanical failure, is used. The change in elastic properties due to microcrack damage calculated from the theoretical model is compared with the experimental results for determination of the applicability of damage theory. It is shown that two independent experimental methods (bulk wave and surface wave) give the same results for shear moduli of damaged ceramics. The experimental results aagree reasonably well with the moduli predicted from the cracked solid model.

Chu, Y. C.↗

NASA NTRS1996

Sol-gel Technology and Advanced Electrochemical Energy Storage Materials

Advanced materials play an important role in the development of electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. The sol-gel process is a versatile solution for use in the fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. This processing technique is particularly useful in producing porous materials with high surface area and low density, two of the most desirable characteristics for electrode materials. In addition,the porous surface of gels can be modified chemically to create tailored surface properties, and inorganic/organic micro-composites can be prepared for improved material performance device fabrication. Applications of several sol-gel derived electrode materials in different energy storage devices are illustrated in this paper. V2O5 gels are shown to be a promising cathode material for solid state lithium batteries. Carbon aerogels, amorphous RuO2 gels and sol-gel derived hafnium compounds have been studied as electrode materials for high energy density and high power density electrochemical capacitors.

Chung-tse Chu↗

NASA NTRS1999

The Features of Self-Assembling Organic Bilayers Important to the Formation of Anisotropic Inorganic Materials in Microgravity Conditions

There is a growing need for inorganic anisotropic particles in a variety of materials science applications. Structural, optical, and electrical properties can be greatly augmented by the fabrication of composite materials with anisotropic microstructures or with anisotropic particles uniformly dispersed in an isotropic matrix. Examples include structural composites, magnetic and optical recording media, photographic film, certain metal and ceramic alloys, and display technologies including flat panel displays. While considerable progress has been made toward developing an understanding of the synthesis of powders composed of monodispersed, spherical particles, these efforts have not been transferred to the synthesis of anisotropic nanoparticles. The major objective of the program is to develop a fundamental understanding of the growth of anisotropic particles at organic templates, with emphasis on the chemical and structural aspects of layered organic assemblies that contribute to the formation of anisotropic inorganic particles.

Talham, Daniel R.↗

NASA NTRS2002

Environment-Conscious Ceramics (Ecoceramics) Technology Received 2001 R&D 100 Award

Since the dawn of human civilization, there has been a delicate balance between the use of resources as human frontiers expanded and the need to have a minimum influence on the ecosystem. The first 200 years of the industrial revolution essentially solved the problem of production. However, the massive production of goods also generated tremendous amounts of byproducts and wastes. In the new millennium, to sustain a healthy life in harmony with nature, it will be extremely important for us to develop various materials, products, and processes that minimize any harmful influence on the environment. Environment-conscious ceramics (ecoceramics) are a new class of materials that can be fabricated with renewable resources (wood) and wood waste material (wood sawdust). Wood is a "lignocellulosic" material formed by the photosynthetic reaction within the needles or leaves of trees. The photosynthesis process uses sunlight to take carbon dioxide from air and convert it into oxygen and organic materials. Wood has been known to be one of the best and most intricate engineering materials created by nature and known to mankind. In addition, natural woods of various types are available throughout the world. On the other hand, wood sawdusts are generated in abundant quantities by sawmills. Environment-conscious ceramic materials, fabricated via the pyrolysis and infiltration of natural wood-derived preforms, have tailorable properties with numerous potential applications. The experimental studies conducted to date on the development of materials based on biologically derived structures indicate that these materials behave like ceramic materials manufactured by conventional approaches. These structures have been shown to be quite useful in producing porous or dense materials having various microstructures and compositions.

Singh, Mrityunjay↗

NASA NTRS2005

The features of self-assembling organic bilayers important to the formation of anisotropic inorganic materials in microgravity conditions

Materials with directional properties are opening new horizons in a variety of applications including chemistry, electronics, and optics. Structural, optical, and electrical properties can be greatly augmented by the fabrication of composite materials with anisotropic microstructures or with anisotropic particles uniformly dispersed in an isotropic matrix. Examples include structural composites, magnetic and optical recording media, photographic film, certain metal and ceramic alloys, and display technologies including flat panel displays. The new applications and the need for model particles in scientific investigations are rapidly out-distancing the ability to synthesize anisotropic particles with specific chemistries and narrowly distributed physical characteristics (e.g. size distribution, shape, and aspect ratio).

Talham, Daniel R.↗

NASA NTRS2012

Development of Matrix Microstructures in UHTC Composites

One of the major issues hindering the use of ultra high temperature ceramics for aerospace applications is low fracture toughness. There is considerable interest in developing fiber-reinforced composites to improve fracture toughness. Considerable knowledge has been gained in controlling and improving the microstructure of monolithic UHTCs, and this paper addresses the question of transferring that knowledge to composites. Some model composites have been made and the microstructures of the matrix developed has been explored and compared to the microstructure of monolithic materials in the hafnium diboride/silicon carbide family. Both 2D and 3D weaves have been impregnated and processed.

Johnson, Sylvia↗

NASA NTRS2016

Post-Flight Assessment of Avcoat Thermal Protection System for the Exploration Flight Test-1

On December 5, 2014 NASA conducted the first flight test of its next generation human-class Orion spacecraft. The flight was called the Exploration Flight Test -1 (EFT-1) which lasted for 4 hours and culminated into a re-entry trajectory at 9 km/s. This flight test of the 5-meter Orion Crew Module demonstrated various sub-systems including the Avcoat ablative thermal protection system (TPS) on the heat shield. The Avcoat TPS had been developed from the Apollo-era recipe with a few key modifications. The engineering for thermal sizing was supported by modeling, analysis, and ground tests in arc jet facilities. This paper will describe a postlfight analysis plan and present results from post-recovery inspections, data analysis from embedded sensors, TPS sample extraction and characterization in the laboratory. After the recovery of the vehicle, a full photographic survey and surface scans of the TPS were performed. The recovered vehicle showed physical evidence of flow disturbances, varying degrees of surface roughness, and excessive recession downstream of compression pads. The TPS recession was measured at more than 200 locations of interest on the Avcoat surface. The heat shield was then processed for sample extraction prior to TPS removal using the 7-Axis Milling machine at Marshall Space Flight Center. Around 182 rectangular TPS samples were extracted for subsequent analysis and investigation. The final paper will also present results of sample analysis. The planned investigation includes sidewall imaging, followed by image analysis to characterize TPS response by quantifying different layers in the char and pyrolysis zones. A full postmortem of the instrumentation and sensor ports will also be performed to confirm no adverse effects due to the sensors themselves. A subset of the samples will undergo structural testing and perform detailed characterization of any cracks and integrity of gore seams. Finally, the material will be characterized with layer-by-layer density measurements and SEM investigations to evaluate material morphology at microstructural level including identification of elements and compounds.

Aerothermodynamics↗