Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “microstructure characterization”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,711 records · Page 95

Multiple Concentric Cylinder Model (MCCM) user's guide

A user's guide for the computer program mccm.f is presented. The program is based on a recently developed solution methodology for the inelastic response of an arbitrarily layered, concentric cylinder assemblage under thermomechanical loading which is used to model the axisymmetric behavior of unidirectional metal matrix composites in the presence of various microstructural details. These details include the layered morphology of certain types of ceramic fibers, as well as multiple fiber/matrix interfacial layers recently proposed as a means of reducing fabrication-induced, and in-service, residual stress. The computer code allows efficient characterization and evaluation of new fibers and/or new coating systems on existing fibers with a minimum of effort, taking into account inelastic and temperature-dependent properties and different morphologies of the fiber and the interfacial region. It also facilitates efficient design of engineered interfaces for unidirectional metal matrix composites.

Williams, Todd O.↗

Micromechanics Based Design/Analysis Codes for Advanced Composites

Advanced high temperature Ceramic Matrix Composites (CMC) hold an enormous potential for use in aero and space related applications specifically for propulsion system components. Consequently, this has led to a multitude of research activities pertaining to fabrication, testing and modeling of these materials. The efforts directed at the development of ceramic matrix composites have focused primarily on improving the properties of the constituents as individual phases. It has, however, become increasingly clear that for CMC to be successfully employed in high temperature applications, research and development efforts should also focus on optimizing the synergistic performance of the constituent phases within the as-produced microstructure of the complex shaped CMC part. Despite their attractive features, the introduction of these materials in a wide spectrum of applications has been excruciatingly slow. The reasons are the high costs associated with the manufacturing and a complete experimental testing and characterization of these materials. Often designers/analysts do not have a consistent set of necessary properties and design allowables to be able to confidently design and analyze structural components made from these composites. Furthermore, the anisotropy of these materials accentuates the burden both on the test engineers and the designers by requiring a vastly increased amount of data/characterization compared to conventional materials.

Mital, Subodh K.↗

Investigation into Interfacial Mixing Behavior of Blown Powder Deposited Inconel 625-Copper Alloy Bimetallic for Improvement of Bimetallic Joint Strength

Use of laser blown powder, directed energy deposition (DED) provides a method for fabrication of bimetallic functional materials for high heat flux applications. However, this relatively new process currently has a low technology readiness level (TRL). Key to increasing the TRL is a better understanding of the factors that control mixing of the bi-metallic materials at the interface. The resulting interfaces in specimens obtained from three vendors were characterized using optical and electron microscopy with electron dispersion spectroscopy in addition to mechanical testing. Based on the range of process parameters and resulting interfaces, a model is being developed to predict interfacial mixing for development of specifications for improved and repeatable microstructures.

Additive Manufacturing↗

Microstructural evolution and precipitation in γ-LiAlO 2 during ion irradiation

Polycrystalline γ-LiAlO 2 pellets were sequentially irradiated with 120 keV He + and 80 keV D 2 + ions to the fluences of 1 × 10 17 and 2 × 10 17 (He + + D + )/cm 2 at 573 K. Additional irradiation was performed to a fluence of 2 × 10 17 (He + + D + )/cm 2 at 773 K. The irradiated pellets were characterized using scanning transmission electron microscopy, time-of-flight secondary ion mass spectrometry, and grazing incidence x-ray diffraction. Lattice damage, amorphization, and fractures are observed with no evidence for the formation of secondary-phase precipitates in the pellets irradiated up to an ion fluence of 2 × 10 17 (He + + D + )/cm 2 at 573 K. In contrast, faceted precipitates with sizes larger than 100 nm formed in a pellet irradiated to 2 × 10 17 (He + + D + )/cm 2 at 773 K. Analyses of the diffraction and composition data suggest that the precipitates have a spinel-type structure, likely a non-stoichiometric LiAl 5 O 8 with Li depletion. This could be an intermediate phase with Li atoms at the octahedral and possibly tetrahedral sites as well. It is speculated that as the dose increases, Li loss will continue and the precipitates will approach a composition of alumina primarily in phases of α-Al 2 O 3 and amorphized Al 2 O 3 .

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Competing Interactions between Mesoscale Length-Scales, Order-Disorder, and Martensitic Transformation in Ferromagnetic Shape Memory Alloys

In the present study, the effects of composition and heat treatments and the resulting microstructural changes on the martensitic transformation and ferromagnetic transition have been investigated in NiCoMnIn metamagnetic shape memory alloys. In this shape memory alloy system, it is observed that upon heat treatments at a wide temperature range, the onset temperature of the martensitic transformation follows a non-monotonic behavior with respect to heat treatment time, and the nature of the non-monotonic behavior is also a function of composition. This behavior cannot be attributed to well-known factors such as precipitation, change in local composition due to the precipitation and/or global degree of order. In this work, a systematic investigation through synthesis, thermal processing and characterization via thermo-physical measurements, transmission electron microscopy and in-situ synchrotron x-ray diffraction experiments has been used to correlate the non-monotonic dependence of the martensitic transformation and ferromagnetic transition temperatures to the evolution of L2 1 domains arising from a order/disorder phase transition. A thermodynamic model for the magneto-structural transition is combined with classical nucleation theory to further ascertain the role of microstructural length-scales on the onset of the martensitic transformation. This work thus provides understanding of the thermodynamic and kinetic factors that can be controlled to tune the coupled magneto-structural transformations in NiCoMnIn metamagnetic shape memory alloys.

36 MATERIALS SCIENCE↗

Microstructural Analysis of Iron-Chromium-Aluminum Samples Exposed to Loca-Type Conditions Followed by Quench

The QUENCH-19 experiment was performed to examine the behavior of FeCrAl-alloy B1236Y3 as a potential nuclear fuel cladding and accident conditions. Over the course of the test, a surrogate bundle achieved a temperature of just over 1400°C. Post-test characterization revealed that the FeCrAl formed a thin layer of aluminum oxide that protected most of the underlying cladding and surrogate fuel pin. However, a few pins were heavily corroded and even destroyed primarily by thermocouple-FeCrAl interactions and subsequent steam, FeCrAl, and ZrO 2 interactions. Absent these effects, it is suggested that FeCrAl’s performance may be acceptable under these conditions.

36 MATERIALS SCIENCE↗

Characterization of radiation damage effects in high-energy neutrino target graphite using low-energy ions

Exposure of graphite targets to high intensity proton beams at neutrino production facilities causes changes in the target material that can result in a shortened operation lifetime. The dominant factors in this process are currently thought to be mechanical in nature resulting primarily from microstructural effects that lead to thermal and structural changes in bulk material properties. As currently planned beam facilities with increased proton energy and intensity begin to come online it will be important to thoroughly understand these processes, and ideally to be able to predict the effects of new beam designs on target properties. Direct analysis of targets exposed to existing high-energy proton beams is complicated by several factors, such as very limited access to proton beam facilities, high associated costs, irradiation times on the order of months, and the resulting radioactivity of irradiated samples that requires special facilities for post-irradiation examination. Much of the existing literature concerning irradiation damage in graphite has been focused on the needs of the nuclear engineering community, however high-energy proton targets operate in a much different environment. In comparison to graphite irradiated in a nuclear reactor, graphite used in proton beam targets receives a higher dose rate, have greater gas production, and experience short irradiation pulses as opposed to continuous irradiation. Low-energy ion irradiation offers a method of inducing similar levels of radiation damage to high-energy protons while avoiding many of the difficulties and limitations associated with high-energy proton beams and the corresponding activated specimen testing. My research described in this thesis focused on investigating how low-energy ion irradiation could be used to induce the same or similar types of microstructural alteration and mechanical property degradation as that seen in high-energy neutrino production target graphites by varying damage le vels and irradiation temperatures prior to post-irradiation characterisation.

43 PARTICLE ACCELERATORS↗

A comparative study of solute trapping in Fe-(33–45 at%) Cu alloys manufactured by laser directed energy deposition

The high cooling rates in laser directed energy deposition (DED-LB) of alloys lead to substantial amounts of solute trapping as solute atoms cannot diffuse away from the solid/liquid interface before it advances. In some concentrated alloys, this results in supersaturated solid phases that form nanoscale hierarchical microstructures when the solute atoms precipitate out during reheating from subsequent laser passes. We choose the Iron-Copper (Fe-Cu) binary alloy as model system as it is chemically homogeneous in the liquid phase and has negligible solid solubility at room temperature. Two alloys with nominal compositions in atomic (at.) %, Fe67Cu33 and Fe55Cu45, were manufactured using DED-LB. Scanning transmission electron microscopy (STEM), energy dispersive spectroscopy (EDS) and wavelength dispersive spectroscopy (WDS) were used to characterize the nanostructures and heterogeneous chemical compositions. A non-equilibrium solute partitioning model was used to compute the supersaturated chemistries of the constituent phases and validated with experimentally measured compositions. The measured phase compositions of the two alloys were very similar, at roughly 12 at.% Cu and 4 at.% Fe in the α(bcc)-Fe and ε(fcc)-Cu phases respectively, despite having different processing parameters and mechanical behavior. This indicates that the total thermal history, that depends on both the processing parameters and laser scan pattern, plays a stronger role on the final microstructure evolution than just the initial quantity of trapped solute. In addition, we find that current non-equilibrium solute partitioning models applied on the continuum scale fall short of predicting accurate quantitative phase compositions in concentrated alloys, although the qualitative trends are captured correctly.

36 MATERIALS SCIENCE↗

Numerical investigation of thermomechanical response of multiscale porous Ultra-High Temperature Ceramics

Recent advances in Ultra-High Temperature Ceramics (UHTC) manufacturing have permitted the development of multiscale porous UHTC microstructures. Within the target application of hypersonic vehicles, dense UHTCs are suitable for thermal protection on leading edges, whereas porous UHTCs may find a role in providing thermally insulated interfaces for temperature-sensitive interior components. Designing vehicles incorporating porous UHTCs requires a characterization of their thermomechanical properties across the full range of expected operating temperatures spanning –20 °C–2500 °C. This research represents a preliminary study in performing this characterization. Several numerical experiments are performed using a coupled thermomechanical implementation of the Material Point Method to determine the temperature dependence of effective material properties both with and without damage. Furthermore, complex time-dependent boundary conditions derived from known hypersonic flight profiles are simulated in order to probe the various couplings between deformation, damage and heat transfer. It is shown that the model reveals the importance of micro-buckling in determining effective material stiffness and thermal conductivity.

36 MATERIALS SCIENCE↗

Boosting the sodium storage behaviors of carbon materials in ether-based electrolyte through the artificial manipulation of microstructure

The porous carbon blacks rationally designed by a facile yet efficient NH 3 thermal etching route have been investigated as anode materials in an ether-based electrolyte for sodium-ion batteries. The as-synthesized CBN35 carbon black with a 35% weight loss after NH3 thermal etching exhibited a large specific charge capacity of 352 mAh g -1 at 50 mA g -1 and a superior rate capability of 101 mAh g -1 at 16000 mA g -1 , due to its highest microporosity, an appropriate surface area, a desirable microstructure, and a promising hybrid intercalation mechanism. Impressively, even cycled at 1600 mA g -1 over 3200 cycles, an outstanding reversible capacity of 103 mAh g -1 with a negligible 0.0162% capacity loss per cycle can still be achieved. Based on the multimodal characterizations including the structural probes of phase evolution for carbon materials, the electrochemical techniques, and the surface-sensitive XAS measurements, the exceptional electrochemical properties should stem from several merits of modified carbon black system. While the particular microporous structure provides relatively more accessible sodium storage sites, a novel hybrid intercalation mechanism in ether-based electrolyte would incorporate the sodium ion insertion into the disordered structure with the solvated sodium ion species co-intercalation into the graphitic phase. In addition to the diffusion-controlled redox reactions, the noticeable surface-induced pseudocapacitive reactions also significantly contribute to the charge storage upon sodiation and guarantee the rapid migrations of sodium ions/solvated compounds. In conclusion, this system further features a controlled emergence of a robust but thin solid electrolyte interphase layer, which could suppress the side reactions of active electrode with reactive electrolyte, maintain the fragile porous structure upon cycling, and facilitate the migrations of sodium ions and solvated sodium ion compounds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Transformational faulting in Mn 2 GeO 4 from olivine to wadsleyite structure: Implications for physical mechanism of deep-focus earthquakes

High-pressure and temperature deformation experiments interfaced with acoustic emission (AE) monitoring have been conducted to study transformational faulting in Mn 2 GeO 4 olivine, which transforms to the β phase, isostructural to wadsleyite. Metastable Mn 2 GeO 4 olivine exhibits a marked embrittlement behavior at temperatures between 800 and 1100 K, emitting numerous AEs. At each temperature, brittle deformation is characterized by a two-stage process: (1) a “preparation” stage with numerous diffusedly located low-magnitude AEs and large b values (>2), and (2) a failure stage where larger-magnitude AEs form a planar distribution with b values about 1. Microstructure analysis reveals extensive kink band development in olivine grains in the recovered samples. Kink band boundaries (KBBs), with a typical thickness of ∼100 nm, are filled with a nanometric β-Mn 2 GeO 4 “gouge”. A dense array of secondary shear localizations is often present within the kink bands, suggesting significant shear deformation therein. The combined observations suggest that faulting in metastable Mn 2 GeO 4 olivine is a self-similar process, from grain-scale to the sample-scale. Both observed embrittlement behavior and the microstructure of metastable Mn 2 GeO 4 olivine are essentially identical to those in Mg 2 GeO 4 olivine we have reported previously, indicating that the physical mechanism of faulting in metastable olivine is insensitive to the specific crystallographic structure of the high-pressure phase. The low b values (about 1) observed in the faulting process in our experiments are similar to those of deep focus earthquakes in cold subduction zones. Our observed mechanism explains deep focus seismicity in cold metastable mantle wedges, provided that the self-similarity assumption holds to geological scales.

58 GEOSCIENCES↗

Elucidating the mechanical and thermal response of nanotwinned Ni alloys

Transformative advances in nanoscale materials synthesis, characterization and modeling are enabling the synthesis of materials with unprecedent properties and greater understanding of the nanoscale mechanisms that underpin these properties. Nanotwinned Cu alloys have received considerable attention due to their impressive balance of strength and ductility, but they have limited microstructural stability. Recent instantiation of nanotwins in sputter deposited Ni-Mo-W, and several commercial Ni-based superalloys, point to the potential development of a new class of high temperature materials with a very beneficial suite of mechanical and physical properties. The experimental study described in this report was undertaken to elucidate the nanoscale origins of the thermal and mechanical behavior of nanotwinned Ni alloys. Micropillar compression experiments have shown nanotwinned Ni 85 Mo 15-x W x alloys to possess unusually high strengths above 3.5GPa and enhanced microstructural stability. The strength of these nanotwinned alloys is determined by the abrupt formation of shear bands. This study focused on identifying the nanoscale trigger, or triggers, for shear banding in nanotwinned materials using in situ experiments and atomic-scale postmortem analysis. Contrasting and comparing the mechanical response and postmortem nanostructures of “Mo-rich” and “W-rich” nanotwinned specimens elucidated the importance of the lateral motion of easy glide defects that results in erasure of twins and local coarsening of the nanotwinned microstructure. This twin coarsening was then associated with very localized plasticity, strain softening, and shear band formation. The difference between alloys was further studied by considering the role of various material factors: stacking fault energy, coherent twin boundary spacing and flatness, grain size, and the interactions of solute atoms with twin and grain boundaries. The effect of alloy composition and sputtering power and temperature were also investigated and used to control twin spacing and geometry. Combined with atomic-scale simulations, these experiments insights should allow us to identify strategies for achieving concomitant ultrahigh strength and ductility in nanotwinned Ni alloys. In parallel but synergistic studies, our work was buoyed by collaborative state-of-the-art nanoscale orientation and strain mapping at the DOE National Center for Electron Microscopy (NCEM). For example, novel 4D-STEM techniques were used to acquire nanoscale strain maps. The extremely fine twin spacing limited our measurements of atomic-scale thermal expansion within twins, but recent results from NCEM suggest that it will soon be possible to conduct such measurements and to unravel the origins of the novel thermal expansion characteristics of nanotwinned Ni alloys.

36 MATERIALS SCIENCE↗

Interfaces in polymer, ceramic, and metal matrix composites; Proceedings of the Second International Conference on Composite Interfaces (ICCI-II), Cleveland, OH, June 13-17, 1988

The present conference on interfacial factors in advanced composite materials discusses such topics in their development status and properties as silane coupling, the electrochemical and plasma-surface treatment of carbon fibers, fiber surface-analytical techniques, polymer molecular scale characterization by atom-probe field-ion microscopy, the study of carbon fiber-epoxy resin interface interactions by means of labeling techniques, and the surface tailoring of SiC by ion implantation. Also discussed are developments in laser light-scattered photoelasticity, microstructural evolutions under heat treatment and radiation damage, TEM for composites, the interfaces of carbon fiber-reinforced Al composites, the influence of the interface on macroscopic composite properties, and the status of the theoretical understanding of composite interfaces.

Ishida, Hatsuo↗

Mechanical Behavior of a Hi-Nicalon(tm)/SiC Composite Having a Polycarbosilane Derived Matrix

Polymer infiltration of a rigidized preform, followed by pyrolysis to convert the polymer to a ceramic, potentially offers a lower cost alternative to CVD. It also offers more moderate temperature requirements than melt infiltration approaches, which should minimize potential fiber damage during processing. However, polymer infiltration and pyrolysis results in a more microcracked matrix. Preliminary mechanical property characterization, including elevated temperature (1204 C) tensile, 500 h stress rupture behavior and low cycle fatigue, was conducted on Hi-Nicalon (TM)/Si-C-(O) composites having a dual layer BN/SiC interface and a matrix derived by impregnation and pyrolysis of allylhydridopolycarbosilane (AHPCS). Microstructural evaluation of failure surfaces and of polished transverse and longitudinal cross sections of the failed specimens was used to identify predominant failure mechanisms. In stress rupture testing at 1093 C, the failure was interface dominated, while at 1204 C in both stress rupture and two hour hold/fatigue tests failure was matrix dominated, resulting in specimen delamination.

Hurwitz, Frances I.↗

Development of an Effective Finite-rate Oxidation Model for NuSil-coated Charred Carbon Preform Ablators

Recently, a detailed effective finite-rate surface chemistry model was developed for the oxidation of FiberForm [1] using the molecular beam experimental data of Poovathingal et al., [2]. FiberForm is the major building block of the thermal protection system (TPS) material Phenolic Impregnated Carbon Ablator (PICA), commonly used by NASA. The surface chemistry model consists of detailed surface reaction mechanisms such as adsorption, desorption, and several types of Langmuir-Hinshelwood (LH) reactions to characterize the oxygen-carbon interactions at the surface. This model provides excellent agreement with the experimental data for oxidation product compositions and corresponding translational energy distributions. Further, an effective oxidation model was constructed that captures the equivalent interaction of oxygen inside the microstructure (including multiple surface collisions) via a modified reactivity for a smooth wall boundary condition. This enables the use of this model directly into Computational Fluid Dynamics (CFD) codes and Material Response (MR) codes to accurately simulate the gas–surface interactions within FiberForm without using the detailed micro-structure. However, this effective model is valid only for the virgin FiberForm. As the TPS material undergoes ablation, the preform carbon burns and turns into char. In addition, PICA is also coated with a protective silicon coating called NuSil for the purpose of mitigating the spread of phenolic dust, and limit contamination during clean room operations. Fig. 1 shows a X-ray microtomography image of a charred NuSil-coated PICA. The NuSil layer introduces species containing silicon into the product mixture. Further, the reactivity of the carbon within the char layer is different from the virgin FiberForm as shown in Fig. 2. Recently a new set of molecular beam experiments were performed on this NuSil-coated TPS material [3] with the same type of oxygen beam used in the previous experiments. Using the latest experimental data, the previously developed effective model will be extended to account for the charred carbon as well as the NuSil coating. Finally, this new effective model with three phases – preform carbon, char, and NuSil; will be compared and validated against the experimental product compositions.

K Swaminathan Gopalan↗

Microstructure–Property Correlation in a Laser Powder Bed Fusion Processed High-Strength AF-9628 Steel

Laser powder bed fusion additive manufacturing (LPBF-AM) of a low-alloy, high-performance AF-9628 steel results in exceptionally high strength and good ductility. The reasons for such mechanical properties are investigated through detailed microscopy performed at several length scales. Thus, the characterization of melt pool, porosity, grain morphology, phases, and dislocations is performed in the as-printed material. The as-printed material consists of only 0.004 vol% of uniformly distributed porosity, single-phase martensitic laths with an average lath size of ≈2.5 μm, the absence of carbides indicating interstitial trapping of C atom, and high dislocation density in the martensitic laths. Experimental data through microscopy are then fed in analytical models for calculating strengthening contributions from various strengthening mechanisms. Calculated yield strength agrees well with experimentally determined value, and therefore, activation of various strengthening mechanisms is established in as-printed AF-9628.

36 MATERIALS SCIENCE↗

Enhanced Electrochemical Performance of Disordered Rocksalt Cathodes Enabled by a Graphite Conductive Additive

Cobalt-free cation-disordered rocksalt (DRX) cathodes are a promising class of materials for next-generation Li-ion batteries. Although they have high theoretical specific capacities (>300 mA h/g) and moderate operating voltages (~3.5 V vs Li/Li + ), DRX cathodes typically require a high carbon content (up to 30 wt %) to fully utilize the active material which has a detrimental impact on cell-level energy density. To assess pathways to reduce the electrode’s carbon content, the present study investigates how the carbon’s microstructure and loading (10–20 wt %) influence the performance of DRX cathodes with the nominal composition Li 1.2 Mn 0.5 Ti 0.3 O 1.9 F 0.1 . While electrodes prepared with conventional disordered carbon additives (C65 and ketjenblack) exhibit rapid capacity fade due to an unstable cathode/electrolyte interface, DRX cathodes containing 10 wt % graphite show superior cycling performance (e.g., reversible capacities ~260 mA h/g with 85% capacity retention after 50 cycles) and rate capability (~135 mA h/g at 1000 mA/g). Furthermore, a suite of characterization tools was employed to evaluate the performance differences among these composite electrodes. Overall, these results indicate that the superior performance of the graphite-based cathodes is largely attributed to the: (i) formation of a uniform graphitic coating on DRX particles which protects the surface from parasitic reactions at high states of charge and (ii) homogeneous dispersion of the active material and carbon throughout the composite cathode which provides a robust electronically conductive network that can withstand repeated charge–discharge cycles. Overall, this study provides key scientific insights on how the carbon microstructure and electrode processing influence the performance of DRX cathodes. Based on these results, exploration of alternative routes to apply graphitic coatings is recommended to further optimize the material performance.

25 ENERGY STORAGE↗

Roll-to-roll production of catalyst coated membranes for low-temperature electrolyzers

Here we demonstrate a roll-to-roll (R2R) process for direct coating of anode catalyst layers on a polymer electrolyte membrane for low-temperature water electrolysis. To develop this process, we studied catalyst ink formulation, ink-membrane interactions, and coating quality. The catalyst inks were a mixture of iridium oxide (IrO2) and Nafion in a water and alcohol dispersion medium. The type of alcohol (methanol, ethanol, propanols) and water-to-alcohol ratio were varied to determine their influence on membrane swelling, dispersion quality, and coatability. Interactions of the ink dispersion medium with the membrane were characterized using sessile-drop contact-angle measurements. These measurements show that the ratio of water to alcohol has a strong influence on how rapidly the dispersion media is absorbed by the membrane. Rheology of the catalyst inks was measured to understand the microstructure of the catalyst particles in the ink. This analysis found that 1-propanol leads to better dispersion of the IrO2 particles than ethanol. Small-scale coating samples were prepared to understand coating uniformity and formation of irregularities. Subsequently, two water/1-propanol ratios (90:10 and 75:25) were down-selected for large-scale R2R slot die coating. The R2R catalyst-coated membrane (CCM) coating process increased catalyst layer production throughput by over 500x compared to our standard lab-scale spray coating. The CCMs obtained from this process were tested as single-cell membrane electrode assemblies. They exhibited a cell voltage of 1.91 V at a current density of 2 A/cm2, which is comparable to spray-coated CCMs. In conclusion, the work presented here demonstrates a continuous, scalable manufacturing process that eliminates the need for the decal transfer step typically used in CCM production.

42 ENGINEERING↗