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At least 775 records · Page 43

Three-dimensional nucleation and growth of deformation twins in magnesium

At two-thirds the weight of aluminum, magnesium alloys have the potential to reduce the fuel consumption of transportation vehicles. These advancements depend on our ability to optimize the desirable versus undesirable effects of deformation twins, which are three-dimensional (3D) microstructural domains that form under mechanical stresses. Previously only characterized through surface or thin-film measurements, we here present 3D in situ characterization of deformation twinning inside an embedded grain over mesoscopic fields of view using dark-field x-ray microscopy supported by crystal plasticity finite element analysis. The results revealed the role of triple junctions on twin nucleation and the sequence and irregularity of twin growth and showed that twin-grain junctions, twin-twin junctions, and twin boundaries were the sites of localized dislocation accumulation.

Lee, Sangwon [Univ. of Michigan, Ann Arbor, MI (Un↗

Catalytic water splitting kinetics and optimization

This project was motivated primarily by the opportunity of turning photocatalysis into a cost efficient hydrogen generation method for domestic energy and chemical production, and by the need to provide detailed mechanisms of photocatalytic reactions of broad scientific and technological interest. Specifically, we focused on the development of a new technique for analysis of (photo)catalytic reaction mechanisms to guide photocatalyst design. Our approach was based on applying velocity map imaging (VMI) to surface catalyzed reactions in order to identify photocatalytic reaction products, intermediates, and relate these to photocatalyst composition, dimensions, size and other characteristics. By coupling VMI with other spectroscopic and microstructural characterization, we aimed to reveal the features that limit performance of photocatalysis. As a first step to achieve this goal, we constructed a custom VMI microscope specifically designed for investigation of surface photocatalytic reactions and validated it’s design using a photodissociatinon of MnBr(CO) 5 adsorbed on a metallic surface. Using both 230 nm and 266 nm pulsed laser excitations, we observed that there are likely three main pathways for photodissociation of Mn(CO)5Br: from the gas phase, the surface, and ejected Mn complex from the surface increasing the gas phase concentration.

08 HYDROGEN↗

Effects of temperature, thermal exposure, and fatigue on an alumina/aluminum composite

An experimental investigation of the mechanical properties and microstructure of an aluminum matrix/polycrystalline alumina fiber composite material is discussed. The effects of fabrication, isothermal exposure (up to 10,000 hours at 590 K), thermal cycling (6000 cycles between 200 K and 590 K), fatigue (1,000,000 tension-tension cycles) were determined by mechanical testing and metallurgical analysis. The fabrication process severely degraded the fiber strength by reducing the alumina to a nonstoichiometric form and quenching in the resultant vacancies and stress fields. However, isothermal exposure, thermal cycling, and fatigue cycling all restored the fiber strength by enhancing vacancy annihilation. Comparison of the as-fabricated material with other aerospace materials shows that it is an attractive candidate for select applications. Long duration isothermal exposure weakened the matrix by overaging and through the diffusional loss of lithium to a surface reaction forming lithium carbonate. Thermal cycling initiated cracks in the matrix and fibers. Tension-tension fatigue cycling caused no apparent damage to the as-fabricated material but in fact, strengthened it to the rule-of-mixtures value. Fatigue cycling after thermal exposure did have a cumulative damage effect.

Olsen, G. C.↗

A study of microstructural characteristics of Ni-based superalloys at high temperatures

The microstructural characteristics of the Ni-based superalloy MAR-M245(Hf) which is used in manufacturing the components of the Space Shuttle main engine are studied. These superalloys need optimum heat treatment to get the best results. To find out the optimum heat treatment, the techniques of differential thermal analysis (DTA) and the optical photomicrographs were utilized. In the first phase, the existing experimental equipment like cutting, grinding/polishing machines and metallurgical microscope were set up to cut/polish and take the photomicrographs. In the beginning of the project a Perkin Elmer differential thermal analyzer DTA1700 along with a temperature programmed and the needed computer interface was procured and made operational. In the second year a Leitz Metallux-3 hot state research microscope was also procured and installed for in-situ observation of the superalloy samples. The hot stage when tested for the first time alloyed the thermocouple with the Tantalum heating element and has now been installed. Samples of MAR-M246(Hf), MAR-M247, Waspaloy, Udimet-41, CMSX-3, and CMSX-3 (Polycrystalline and single crystals) were studied using a differential thermal analyzer and the results are reported. Photomicrographs of the Ni-based superalloy MAR-M246 (Hf) were recorded before and after heat treatment at certain temperatures. More heat treatments need to be done before a final inference can be reached.

Lal, Ravindra B.↗

Transformation to Ni5Al3 in a 63.0 at. pct Ni-Al alloy

Microstructures of 63 at. pct P/M Ni-Al alloys with a composition close to the stoichiometry of the Ni5Al3 phase were investigated using homogenized and quenched specimens aged at low temperatures for various times. Results of analyses of XRD data and electron microscopy observations were used for quantitative phase analysis, performed to calculate the (NiAl + Ni5Al3)/Ni5Al3 phase boundary locations. The measured lattice parameters of Ni5Al3 phase formed at 823, 873, and 923 K indicated an increase in tetragonality of the phase with increasing nickel content.

Khadkikar, P. S.↗

Lamellar Spacing Selection in Al-Si Eutectic System: a Theoretical Investigation

It is well known that irregular eutectics such as Al-Si and Fe-C exhibit larger lamellar spacings and undercoolings compared to the predictions made by the Jackson and Hunt (JH) theory. In this paper, we reexamine the JH theory and relax some of the assumptions used in that treatment. The modified theoretical model has enhanced capabilities to predict the lamellar spacing in both regular and irregular eutectics. For the Al-Si system in particular we identified two different spacing selection mechanisms:a) for a particular growth rate, a nearly isothermal interface can be achieved at a unique minimum spacing lambda(sub I); b) the average spacing in the microstructure (lambda(sub av) greater than lambda(sub I)) is essentially dictated by the undercooling of the faceted phase. Based on the modified theoretical model a semi-empirical expression has been developed to account for the influence of the temperature gradient. Application of a Mullin and Sekerka type stability analysis for eutectics will also be presented and the results compared to the modified JH model. It will be shown that the both theoretical approaches are in good agreement with each other and also with the published experimental measurements.

Catalina, Adrian V.↗

Designing Gamma TiAl Alloys (K5 Based) for Use at 840 C and Above

The objective of this program was to investigate how carbon additions and Al content variation affects RT tensile properties and creep performance in gamma TiAl alloys. On the basis of the results from the work four alloys were selected within the composition range of Ti-(44.7-47.0) Al-(1.0-1.7)Cr-3.0Nb-0.2W-0.2B-(0.23-0.43)C-(0, 0.2)Si. Through extensive annealing/aging experiments, detailed observations of microstructure evolution, property measurements and analyses, comprehensive understanding was made in the carbide formation process. It was found that creep properties depend on the distribution of carbide particles, which is controlled not only by the aging process but also the amount ratio fo Al and carbon. From the results and analysis, new creep-resistant alloy compositions are suggested for further development.

Kim, Young-Won↗

Examination of the Atomic Pair Distribution Function (PDF) of SiC Nanocrystals by In-situ High Pressure Diffraction

Key properties of nanocrystals are determined by their real atomic structure, therefore a reasonable understanding and meaningful interpretation of their properties requires a realistic model of the structure. In this paper we present an evidence of a complex response of the lattice distances to external pressure indicating a presence of a complex structure of Sic nanopowders. The experiments were performed on nanocrystalline Sic subjected to hydrostatic or isostatic pressure using synchrotron and neutron powder diffraction. Elastic properties of the samples were examined based on X-ray diffraction data using a Diamond Anvil Cell (DAC) in HASYLAB at DESY. The dependence'of the lattice parameters and of the Bragg reflections width with pressure exhibits a ha1 nature of the properties (compressibilities) of the powders and indicates a complex structure of the grains. We interpreted tws behaviour as originating from different elastic properties of the grain interior and surface. Analysis of the dependence of individual interatomic distances on pressure was based on in-situ neutron diffraction measurements done with HbD diffractometer at LANSCE in Los Alamos National Laboratory with the Paris-Edinburgh cell under pressures up to 8 GPa (Qmax = 26/A). Interatomic distances were obtained by PDF analysis using the PDFgetN program. We have found that the interatomic distances undergo a complex, non-monotonic changes. Even under substantial pressures a considerable relaxation of the lattice may take place: some interatomic distances increase with an increase in pressure. We relate this phenomenon to: (1), changes of the microstructure of the densified material, in particular breaking of its fractal chain structure and, (2), its complex structure resembling that of a material composed of two phases, each with its distinct elastic properties.

Grzanka, E.↗

Pilot Study: Unique Response of Bone Tissue During an Investigation of Radio-Adaptive Effects in Mice

PURPOSE: We obtained bone tissue to evaluate the collateral effects of experiments designed to investigate molecular mechanisms of radio-adaptation in a mouse model. Radio-adaptation describes a process by which the prior exposure to low dose radiation can protect against the toxic effect of a subsequent high dose exposure. In the radio-adaptation experiments, C57Bl/6 mice were exposed to either a Sham or a priming Low Dose (5 cGy) of Cs-137 gamma rays before being exposed to either a Sham or High Dose (6 Gy) 24 hours later. ANALYSIS: Bone tissue were obtained from two experiments where mice were sacrificed at 3 days (n=3/group, 12 total) and at 14 days (n=6/group, 24 total) following high dose exposure. Tissues were analyzed to 1) evaluate a radio-adaptive response in bone tissue and 2) describe cellular and microstructural effects for two skeletal sites with different rates of bone turnover. One tibia and one lumbar vertebrae (LV2), collected at the 3-day time-point, were analyzed by bone histomorphometry and micro-CT to evaluate the cellular response and any evidence of microarchitectural impact. Likewise, tibia and LV2, collected at the 14-day time-point, were analyzed by micro-CT alone to evaluate resulting changes to bone structure and microarchitecture. The data were analyzed by 2-way ANOVA to evaluate the effects of the priming low dose radiation, of the high dose radiation, and of any interaction between the priming low and high doses of radiation. Bone histomorphometry was performed in the cancellous bone (aka trabecular bone) compartments of the proximal tibial metaphysis and of LV2. RESULTS: Cellular Response @ 3 Days The priming Low Dose radiation decreased osteoblast-covered bone perimeter in the proximal tibia and the total cell density in the bone marrow in the LV2. High Dose radiation, regardless of prior exposure to priming dose, dramatically reduced total cell density in bone marrow of both the long bone and vertebra. However, in the proximal tibia, High Dose radiation increased the osteoclast-covered bone perimeters, the density of adipocytes in bone marrow, and the area of bone marrow occupied by fat cells -- while in the LV2, adipocytes were rare and not stimulated by High Dose radiation. In an unexpected response, High Dose radiation dramatically increased (10-fold) osteoblast-covered bone perimeter in the LV2.

Sibonga, J. D.↗

Establishing and Maintaining the Digital Thread of Additively Manufactured Materials and Applications

Additive Manufacturing (AM) and Integrated Computational Materials Engineering (ICME) are complementary enabling technologies for design and manufacturing of “fit-for-purpose” materials. Both technologies will impact rapid material design, reduction in cost- and time-to-market for new applications, and discovery and implementation of new materials. An ICME approach to design, however, requires experimentally validated material models at multiple length and time scales, an integrated framework that can connect analysis tools with one another to ensure the digital thread of an application is maintained, and the manufacturing (e.g., AM) capability to leverage processing-structure-property-performance (PSPP) relationships to achieve spatially varying material properties where desired. AM enables the implementation of the design of an optimized, spatially varying microstructure through careful selection of the processing parameters used during an additively manufactured build. In order to establish these PSPP relations, a large amount of data is necessary, and that data must be properly captured, analyzed and maintained in an information management system that can establish the required traceability between various aspects of the design process to ensure an application’s digital thread is maintained (from design to end of life). Such an information management system must be able to capture feedstock material pedigree, resulting microstructure from various build parameters, subsequent mechanical properties derived from testing, developed material models, and enable spatial variations in material assignment in an engineering application. Furthermore, the information management system should be easily integrated with traditionally engineered materials in a single, centralized platform to enable an ICME optimization tool to explore both types of manufacturing processes. At NASA GRC, a robust, 21st century materials information management system has been previously developed with a focus towards enabling ICME. In this work, GRC’s ICME schema is extended to accommodate additively manufactured materials, enabling storage of both traditionally and additively manufactured materials in the same construct. The methodology for properly capturing additively manufactured materials across the entire material lifecycle is presented, following the previously established database best practices, as a potential framework for establishing PSPP relationships for additively manufactured materials and applying them to engineering applications.

Data management↗

Characterization of Fuel Cladding Chemical Interaction on a High Burnup U-10Zr Metallic Fuel via Electron Energy Loss Spectroscopy Enhanced by Machine Learning

Fuel cladding chemical interaction (FCCI) is one of the main performance limiting factors for metallic nuclear fuels. The interaction destabilizes the martensitic microstructure and deteriorates mechanical properties of HT-9 cladding. The detection of low atomic number elements (Z<10) and overlapping of elemental peaks can be problematic in interpreting energy dispersive X-ray spectroscopy (EDS) data. Electron energy loss spectroscopy (EELS) provides precise elemental edge energy values and can detect elements with a low atomic number. This work utilizes EELS to study the distribution of lanthanides and light elements at the interaction region. The sample was prepared from the FCCI region of a U-10Zr (wt.%) solid fuel with HT-9 cladding, irradiated to a burnup of 13.2 at.%. Processing the EELS data included three major steps: 1) enhance the signal to noise ratio by denoising the spectrum with principal component analysis (PCA) method, removing background and performing deconvolution; 2) identify chemical elements with core energy loss edges; 3) confirm different phases using a popular machine learning method, K-means. This work presents qualitative assessment of lanthanides and light elements like carbon (C) and oxygen (O) enhanced by the application of machine learning algorithms. By comparing with EDS elemental maps, EELS provides higher resolution chemical maps, reveals the distribution of carbon at the interaction region supporting the formation of zirconium carbide, a rind-like microstructure feature that was proposed to mitigate the chemical interaction. Furthermore, the plasmon peak map was also found to indicate an energy shift associated with the formation of phases/compounds. K-means clustering method was used on the processed electron energy loss (EEL) spectrum to automatically reveal different phases. The resulting clustered maps from K-means clustering align well with elemental maps confirming certain phases, especially Fe-Ce and Zr-C, in the FCCI region.

EELS↗

Carbon-Binder Optimization for Lithium-Ion Battery Extreme Fast Charge

Battery performance is strongly correlated with electrode microstructure and weight loading of the electrode components. Among them are the carbon-black and binder additives that enhance effective conductivity and provide mechanical integrity. However, these both reduce effective ionic transport in the electrolyte phase and reduce energy density. Therefore, an optimal additive loading is required to maximize performance, especially for fast charging where ionic transport is essential. Such optimization analysis is however challenging due to the nanoscale imaging limitations that prevent characterizing this additive phase and thus quantifying its impact on performance. Herein, an additive-phase generation algorithm has been developed to remedy this limitation and identify percolation threshold used to define a minimal additive loading. Improved ionic transport coefficients from reducing additive loading has been then quantified through homogenization calculation, macroscale model fitting, and experimental symmetric cell measurement, with good agreement between the methods. Rate capability test demonstrates capacity improvement at fast charge at the beginning of life, from 37% to 55%, respectively for high and low additive loading during 6C CC charging, in agreement with macroscale model, and attributed to a combination of lower cathode impedance, reduced electrode tortuosity and cathode thickness.

carbon-binder additives↗

A study of microstructural characteristics of Ni-based superalloys at high temperatures

The microstructural characteristics of the Ni-based superalloy MAR-M246(Hf) which is used in manufacturing the components of the Space Shuttle's main engine have been studied. These superalloys need optimal heat treatment to get the best results. To find the optimum heat treatment the technique of differential thermal analysis and the optical photomicrographs are being planned to be utilized. In the first phase, the existing experimental equipment like cutting, grinding/polishing machines and metallurgical microscope have been set up to cut/polish and take the photomicrographs. In the beginning of this year an order was placed for the Leitz Mettalux-3 microscope with a hot stage for in-situ observation of the superalloy samples. The hot stage was tested for the first time, alloying the thermocouple with the Tantulum heating element and has not been installed finally by the supplier. A Perkin Elmer Differential Thermal Analyzer (DTA 1700) was procured in the first year of the project. Samples of MAR-M246(Hf), MAR-M247, Waspaloy, Udimet-41, CMSX-2 and CMSX-3 (polycrystalline and single crystals) have been studied using differential thermal analyzer.

Lal, R. B.↗

Zirconia toughened SiC whisker reinforced alumina composites small business innovation research

The objective of this phase 1 project was to develop a ceramic composite with superior fracture toughness and high strength, based on combining two toughness inducing materials: zirconia for transformation toughening and SiC whiskers for reinforcement, in a controlled microstructure alumina matrix. The controlled matrix microstructure is obtained by controlling the nucleation frequency of the alumina gel with seeds (submicron alpha-alumina). The results demonstrate the technical feasibility of producing superior binary composites (Al2O3-ZrO2) and tertiary composites (Al2O3-ZrO2-SiC). Thirty-two composites were prepared, consolidated, and fracture toughness tested. Statistical analysis of the results showed that: (1) the SiC type is the key statistically significant factor for increased toughness; (2) sol-gel processing with a-alumina seed had a statistically significant effect on increasing toughness of the binary and tertiary composites compared to the corresponding mixed powder processing; and (3) ZrO2 content within the range investigated had a minor effect. Binary composites with an average critical fracture toughness of 6.6MPam sup 1/2, were obtained. Tertiary composites with critical fracture toughness in the range of 9.3 to 10.1 MPam sup 1/2 were obtained. Results indicate that these composites are superior to zirconia toughened alumina and SiC whisker reinforced alumina ceramic composites produced by conventional techniques with similar composition from published data.

Loutfy, R. O.↗

Development and Characterization of the Bonding and Integration Technologies Needed for Fabricating Silicon Carbide Based Injector Components

Advanced ceramic bonding and integration technologies play a critical role in the fabrication and application of silicon carbide based components for a number of aerospace and ground based applications. One such application is a lean direct injector for a turbine engine to achieve low NOx emissions. Ceramic to ceramic diffusion bonding and ceramic to metal brazing technologies are being developed for this injector application. For the diffusion bonding technology, titanium interlayers (coatings and foils) were used to aid in the joining of silicon carbide (SiC) substrates. The influence of such variables as surface finish, interlayer thickness, and processing time were investigated. Electron microprobe analysis was used to identify the reaction formed phases. In the diffusion bonds, an intermediate phase, Ti5Si3Cx, formed that is thermally incompatible in its thermal expansion and caused thermal stresses and cracking during the processing cool-down. Thinner interlayers of pure titanium and/or longer processing times resulted in an optimized microstructure. Tensile tests on the joined materials resulted in strengths of 13-28 MPa depending on the SiC substrate material. Nondestructive evaluation using ultrasonic immersion showed well formed bonds. For the joining technology of brazing Kovar fuel tubes to silicon carbide, preliminary development of the joining approach has begun. Various technical issues and requirements for the injector application are addressed.

Halbig,Michael C.↗

Eutectic Experiment Development for Space Processing

A ground base test plan and a specimen evaluation scheme have been developed for the aluminum-copper eutectic solidification experiment to be run in the M518 multipurpose electric furnace during the Skylab mission. Besides thermal and solidification studies a detailed description is given of the quantitative metallographic technique which is appropriate for characterizing eutectic structures. This method should prove a key tool for evaluating specimen microstructure which is the most sensitive indicator of changes produced during solidification. It has been recommended that single grain pre-frozen eutectic specimens be used to simplify microstructural evaluation and to eliminate any porosity in the as-cast eutectic specimens. High purity (99.999%) materials from one supplier should be employed for all experiments. Laboratory studies indicate that porosity occurs in the MRC as-cast eutectic ingots but that this porosity can be eliminated by directional freezing. Chemical analysis shows that the MRC ingots are slightly Al rich and contain about .03% impurity. Because of the impurity content the lower cooldown rate (1.2 C/min) should be used for eutectic freezing if MRC material is used in the M518 furnace.

Hopkins, R. H.↗

Active Metal Brazing and Adhesive Bonding of Titanium to C/C Composites for Heat Rejection System

Robust assembly and integration technologies are critically needed for the manufacturing of heat rejection system (HRS) components for current and future space exploration missions. Active metal brazing and adhesive bonding technologies are being assessed for the bonding of titanium to high conductivity Carbon-Carbon composite sub components in various shapes and sizes. Currently a number of different silver and copper based active metal brazes and adhesive compositions are being evaluated. The joint microstructures were examined using optical microscopy, and scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS). Several mechanical tests have been employed to ascertain the effectiveness of different brazing and adhesive approaches in tension and in shear that are both simple and representative of the actual system and relatively straightforward in analysis. The results of these mechanical tests along with the fractographic analysis will be discussed. In addition, advantages, technical issues and concerns in using different bonding approaches will also be presented.

Singh, M.↗

Post STS-134 Evaluation of Main Flame Deflector Witness Materials

NASA and USA design engineers submitted witness materials from the solid rocket booster (SRB) main flame deflector for evaluation after the launch of STS-134. The following items were submitted for analysis: 1018 steel witness rods 304 stainless steel caps, tungsten pistons, and A-286 piston sleeves. All of the items were photographed in order to document their condition after the launch of STS-134. All of the items were dimensionally measured in order to determine the amount of material lost during launch. Microstructural changes were observed in the 1018 witness rod metallographic samples due to the heat of the launch

Long, Victoria↗