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At least 163 records · Page 9

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DOE OSTI2022

Resolving the Martensitic Transformation in Q&P Steels In-Situ at Dynamic Strain Rates Using Synchrotron X-ray Diffraction

Herein the dynamic deformation response of two quenching and partitioning (Q&P) steels was investigated using a high strain rate tension pressure bar and in-situ synchrotron radiography and diffraction. This allowed for concurrent measurements of the martensitic transformation, the elastic strains/stresses on the martensite and ferrite, and the bulk mechanical behavior. The steel with the greater fraction of ferrite exhibited greater ductility and lower strength, suggesting that dislocation slip in ferrite enhanced the deformability. Meanwhile, the kinetics of the martensitic transformation appeared similar for both steels, although the steel with a greater ferrite fraction retained more austenite in the neck after fracture.

36 MATERIALS SCIENCE↗

NASA NTRS2018

A Screening Method Using Pulsed-Power Combined with Infrared Imaging to Detect Pattern Defects in Bulk Metal Foil or Thin Film Resistors

Bulk metal foil and thin film resistors occasionally contain localized defects within the etched resistor pattern. Common defects of this type include in-line constrictions referred to as notches, unremoved resistor material bridges between adjacent pattern lines, and embedded non-conductive particles in the resistor material. Such defects are prone to fracture due to thermomechanical fatigue during powered operation, especially power cycling, resulting in positive resistance change and open circuit failure modes. Common screening methods of optical microscopy, short time overload power tests (e.g., 6.25x rated power for 5 seconds) and burn-in (e.g., 1.5x rated power for 100 hours) are useful, but they are not always effective at removing devices with such defects. An improved method has been developed to screen for localized resistor pattern defects. The method involves the application of brief, high power electrical pulses at a low duty cycle while inspecting the resistor with a high resolution, high speed infrared camera. The following test conditions were found to be suitable for this purpose: 6.25x rated power, 1 to 5 pulses, 50 ms pulse width and 10% duty cycle. During the power pulsing, localized constrictions in the resistor pattern are identifiable as hot spots via the infrared camera. Reject criteria can be established based on observations of hot spots. To assess its effectiveness, a total of two hundred eighty (280) surface mount foil resistors (40 each from 7 different lots) were screened using this infrared technique. The screening identified twenty-nine (29) resistors with significant hot spots in the resistor pattern. All 280 resistors were then subjected to an industry standard 10,000 hour life test at 1x rated power at 70°C with power cycled for 90 minutes on and 30 minutes off. During life testing, three resistors exhibited positive resistance change failure mode. All three failures were due to thermomechanical fatigue failure of localized bridge defects at the locations identified via infrared screening. The results of this evaluation illustrate the benefits of the pulsed-power infrared detection screening technique to identify reliability suspect foil or thin film resistors that may escape common screening methods.

screening↗

NASA NTRS2018

A Screening Method Using Pulsed-Power Combined with Infrared Imaging to Detect Pattern Defects in Bulk Metal Foil or Thin Film Resistors

screening↗

NASA NTRS2015

Fracture Growth Testing of Titanium 6AL-4V in AF-M315E

The Green Propellant Infusion Mission (GPIM) will demonstrate the performance of AF-M315E monopropellant in orbit. Flight certification requires a safe-life analysis of the titanium alloy fuel tank to ensure inherent flaws will not cause failure during the design life. Material property inputs for this analysis require testing to determine the stress intensity factor for environmentally-assisted cracking (K (sub EAC)) of Ti 6Al-4V in combination with the AF-M315E monopropellant. Testing of single-edge notched specimens SE(B) representing the bulk tank membrane and weld material were performed in accordance with ASTM E1681. Specimens with fatigue pre-cracks were loaded into test fixtures so that the crack tips were exposed to the monopropellant at 50 degrees Centigrade for a duration of 1,000 hours. Specimens that did not fail during exposure were opened to inspect the crack surfaces for evidence of crack growth. The threshold stress intensity value, KEAC, is the highest applied stress intensity that produced neither a failure of the specimen during the exposure nor showed evidence of crack growth. The threshold stress intensity factor of the Ti 6Al-4V forged tank material when exposed to AF-M315E monopropellant was found to be at least 22.0 kilopounds per square inch. The stress intensity factor of the weld material was at least 31.3 kilopounds per square inch.

AF-M315E↗

DOE OSTI2023

Gradient nanostructuring via compositional means

Nanocrystalline metals are inherently unstable against thermal and mechanical stimuli, commonly resulting in significant grain growth. Also, while these metals exhibit substantial Hall-Petch strengthening, they tend to suffer from low ductility and fracture toughness. With regard to the grain growth problem, alloying elements have been employed to stabilize the microstructure through kinetic and/or thermodynamic mechanisms. And to address the ductility challenge, spatially-graded grain size distributions have been developed to facilitate heterogeneous deformation modes: high-strength at the surface and plastic deformation in the bulk. In the present work, we combine these two strategies and present a new methodology for the fabrication of gradient nanostructured metals via compositional means. Here, we have demonstrated that annealing a compositionally stepwise Pt-Au film with a homogenous microstructure results in a film with a spatial microstructural gradient, exhibiting grains which can be twice as wide in the bulk compared to the outer surfaces. Additionally, phase-field modeling was employed for the comparison with experimental results and for further investigation of the competing mechanisms of Au diffusion and thermally induced grain growth. This fabrication method offers an alternative approach for developing the next generation of microstructurally stable gradient nanostructured films.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Fracture‐Resistant and Thermally Insulating Ultrahigh‐Temperature Carbide Foams

Dense ultrahigh‐temperature ceramics (UHTCs) carbides are recognized as potential materials for thermal protection systems (TPS) owing to properties beyond existing structural materials’ capabilities. Recent advances in UHTCs have enabled the development of multiscale porous microstructures. Herein, it is highlighted that the porosity in UHTCs are no longer treated as a defect but as a functional property specifically tailored for thermal insulation. It is a promising solution to design and fabricate bulk UHTC foams via a freeze‐drying (FD) approach followed by calibrated pressureless spark plasma sintering. Herein, monolithic TaC and HfC UHTC foams and their composite show the partial solid–solution formation of (Ta, Hf)C with porosity ≥50%. TaC–HfC foam (≈80–92 N) shows an intermediate load‐bearing capability compared to monolithic TaC (≈120–135 N) and HfC (≈28–35 N) foams, with no evident cracking on the sample surface. The thermal conductivity of partial solid‐solution TaC–HfC foam increases up to fivefold compared to parent UHTC foams. In the results, solid solutions’ efficacy and pores’ unidirectionality in providing thermal insulation to TaC–HfC while maintaining its high‐load bearing capability are illustrated. In conclusion, the developed technique establishes a new paradigm shift in UHTCs, expanding their potential for TPS in extreme environments.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Revisiting the Origin of Macromolecular Carbon (MMC) in Lunar Basalts 15556 & 10044

Volatile elements influence the geo-chemical evolution of planetary bodies and they are in magmas at every stage, from melting within planetary interiors to eruption at the surface. Analyses of lunar mare basalts supported the hypothesis that lunar mag-mas were depleted in volatiles (H-C-F-Cl-S), relative to their terrestrial analogs [1]. Nevertheless, several early studies of samples returned during the Apollo program proposed that the mare basalt eruptions, including the “fire fountain” eruptions, were propelled by the oxidation of magmatic graphite to CO (and/or CO2) gas [2, 3]. Seminal studies during the 1970’s measured the bulk concentration and isotopic compositions of C from Apollo 11 samples, and identified several carbonaceous compounds, including: (a) gaseous (CO, CO2, and traces of CH4), (b) metallic carbide, and (c) potentially elemental carbon [4-6]. These studies reported a relatively broad range of C contents (~100-400 μg/g) and isotopic values (δC13 = -30 to +20), and suggested that these heterogeneities can be explained by contribution from multiple factors, including: (a) indigenous carbon, (b) solar wind implantation, (c) bombardment and/or meteorite impact, and (d) terrestrial contamination [5,6]. However, unequivocal observations of magmatic graphite in lunar basalts have never been made. Macromolecular carbon (MMC)—graphitic carbon varying from nearly amorphous to highly crystalline varieties—was identified as inclusions hosted by igneous pyroxenes from Martian meteorites and were attributed to being indigenous to Mars [8]. The authors carefully considered the textural and mineralogical relationship of the MMC phases, and concluded that the subset of MMC located within and/or adjacent to cracks, or at a disrupted surface (e.g., cut) were most consistent with terrestrial contamination. The near absence of con-firmed instances of lunar magmatic MMC within the literature [9], combined with the wide range of isotopic values and bulk carbon contents measured in lunar bas-alts begs the question as to whether previously measured carbon is of an indigenous origin, or the result of terrestrial contamination. Using Raman spectroscopy, we have observed MMC in lunar basalts subjected to different forms of anthropogenic modification related to sample preparation including polished sections, sawn surfaces, and fractured surfaces adjacent to sawn sur-faces. We have observed MMC of unknown origin in all of these settings. Here we report the preliminary textural and spectroscopic characteristics of MMC hosted within the groundmass of Apollo 15 (15556) and Apollo 11 basalts (10044) as part of our ongoing investigation of the origin of these carbonaceous materials.

lunar↗

DOE OSTI2022

The effect of stress on the migration of He gas bubbles under a thermal gradient in Fe by phase-field modeling

Here a phase-field model is parameterized to study the effect of elastic stresses on the migration of He gas bubbles in Fe under a temperature gradient. Stresses caused by the gas bubble pressure and residual stress in the Fe matrix are considered. The dependence of He bubble migration velocity on the magnitude of the residual stress, average temperature, temperature gradient, and bubble size is measured. In agreement with a theoretical model based on surface diffusion, simulation results demonstrate that He bubbles move towards the high temperature region with velocities in Fe that are orders of magnitude faster than previously reported in UO 2 . It is found that local stresses in the matrix caused by the He bubble have negligible effect on the bubble migration process; however, residual stresses in the Fe matrix, potentially caused by processing or irradiation, can modestly modify bubble kinetics through pressure dependence of the He diffusion coefficients. Compressive residual stress decreases diffusion coefficients for bulk and surface diffusion mechanisms, thus reducing the migration velocity of the gas bubble. In contrast, tensile residual stress increases the diffusion coefficients, resulting in an increase in the gas bubble migration velocity. This pressure dependence is also consistent with a theoretical model. This phase field model lays the foundation for analysis of bubble coalescence-induced fracture in He bubble-containing steels.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Flexural strength of a conventionally processed and additively manufactured debased 94% alumina

Mechanical strength of a 94 wt% debased alumina was measured using ASTM-C1161 specimens fabricated via conventional and lithography-based ceramic manufacturing (LCM) methods. The effects of build orientation and a 1500°C wet hydrogen fire added to the LCM firing sequence on strength were evaluated. Additionally, a Weibull fit to the conventional flexural specimen data yielded 20 and 356 MPa for the modulus and characteristic strength, respectively. Weibull fits of the data from the LCM specimens yielded moduli between 7.5 and 11.3 and characteristics strengths between 333 and 339 MPa. A Weibull fit to data from LCM specimens subjected to the wet hydrogen fire yielded 14.2 and 376 MPa for the modulus and characteristic strength, respectively. The 95% confidence intervals for all Weibull parameters are reported. Average Archimedes bulk densities of LCM and conventional specimens were 3.732 and 3.730 g/cm 3 , respectively. Process dependent differences in surface morphology were observed in scanning electron microscope (SEM) images of specimen surfaces. SEM images of LCM specimen cross-sections showed alumina grain texture dependent on build direction, but no evidence of porosity concentrated in planes between printed layers. Fracture surfaces of LCM and conventionally processed specimens revealed hackle lines and mirror regions indicative of fracture initiation at the sample surface rather than the interior.

36 MATERIALS SCIENCE↗

NASA NTRS1980

Tribological properties of silicon carbide in metal removal process

This paper reviews material properties of adhesion, friction and wear of single-crystal silicon carbide in contact with metals and alloys involved in a metal removal process such as grinding. The tribological properties in the metal removal processes are divided into properties which remove metal by adhesion between sliding surfaces, and metal removal by silicon carbide sliding against a metal, indenting it, and plowing a series of grooves or furrows. The paper also deals with fracture and deformation characteristics of the silicon carbide surface; the adhesion, friction and metal transfer to silicon carbide is related to the relative chemical activity of the metals. Atomic size and content of alloying elements play a dominant role in controlling adhesion and friction properties of alloys. The friction and abrasive wear decrease as the shear strength of the bulk metal increases.

Miyoshi, K.↗

DOE OSTI2026

Peridynamic modeling of cementitious materials for nuclear waste management

Radioactive and hazardous waste generated from fuel processing plants, nuclear reactors, and hospitals, requires effective management strategies. Cementitious materials are widely applied for these needs, serving as structural materials, reactive barriers, or waste forms. In these applications cracking poses a significant risk to performance, driven by inconsistent shrinkage of the components and the varying strength and permeability of their interfaces. Traditional modeling approaches face challenges in representing the complex fracture behavior of cementitious materials due to the reliance on spatial derivatives and difficulties with mesh generation. Here, to overcome these limitations, we employ peridynamics, a novel continuum mechanics formulation that uses integrals to describe mechanical equilibrium, avoiding discontinuities associated with traditional methods. Through incorporation of a bi-linear softening model and quasistatics, an experimentally validated model for Portland cement concrete samples was created. Mechanical parameters, including compressive strength and elastic modulus were validated and variation due to aggregate packing was evaluated. Additionally, sensitivity analysis of the peridynamic parameters to the bulk material properties was established. The results lay the groundwork for evaluating the impact of unique conditions of cementitious waste forms that can be assessed to improve the reliability of waste management strategies.

Aggregates↗

NASA NTRS1979

Fatigue behavior of SiC reinforced titanium composites

The low cycle axial fatigue properties of 25 and 44 fiber volume percent SiC/Ti(6Al-4V) composites were measured at room temperature and at 650 deg C. The S-N curves for the composites showed no anticipated improvement over bulk matrix behavior at room temperature. Although axial and transverse tensile strength results suggest a degradation in SiC fiber strength during composite fabrication, it appears that the poor fatigue life of the composites was caused by a reduced fatigue resistance of the reinforced Ti(6Al-4V) matrix. The reduced matrix behavior was due, to the presence of flawed and fractured fibers created near the specimen surfaces by preparation techniques and to the large residual tensile stresses that can exist in fiber reinforced matrices. The effects of fatigue testing at high temperature are discussed.

Bhatt, R. T.↗

DOE OSTI2025

Elastomeric Nanocomposite with Solvent‐Free, One Step, In Situ Shear Exfoliation of Graphite to Graphene

A graphene nanoflake (GNF)‐enhanced elastomeric nanocomposite (G‐EMC) is fabricated following an innovative, cost‐effective, single‐step, in situ shear exfoliation (ISE) method from low‐cost bulk material, graphite, where uniform mixing happens simultaneously within the elastomer matrix. Electron microscopy, atomic force microscopy, and photo‐induced force microscopy results show good dispersion of GNFs with exfoliation to a few layers and uniform distribution in the elastomer matrix. X‐ray photoelectron spectroscopy analysis shows less than 1% oxygen‐containing functional groups/impurity, enhanced bonding through the formation of edge sites as fracture occurs across the GNF basal plane, and pi‐pi interactions with newly exfoliated planar basal plane surfaces of the GNFs. Raman spectroscopy results confirm the formation of GNFs with only a few layers of graphene formed by the ISE process. Fabricated 10 wt.% G‐EMC nanocomposites show a 400%–500% increase in strength and fracture toughness. And 35 wt.% G‐EMCs provide an electrical conductivity of 25.64 S m −1 and a sensor gauge factor of 45. The resulting intrinsic piezo resistivity of the fabricated nanocomposite has been exploited to fabricate a multi‐functional wired and wireless sensor for detecting different body movements, speech, human vital functions, solvents, and biomolecules.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Heterogeneous Ice Growth in Micron-Sized Water Droplets Due to Spontaneous Freezing

Understanding how ice nucleates and grows into larger crystals is of crucial importance for many research fields. The purpose of this study was to shed light on the phase and structure of ice once a nucleus is formed inside a metastable water droplet. Wide-angle X-ray scattering (WAXS) was performed on micron-sized droplets evaporatively cooled to temperatures where homogeneous nucleation occurs. We found that for our weak hits ice grows more cubic compared to the strong hits that are completely hexagonal. Due to efficient heat removal caused by evaporation, we propose that the cubicity of ice at the vicinity of the droplet’s surface is higher than for ice formed within the bulk of the droplet. Moreover, the Bragg peaks were classified based on their geometrical shapes and positions in reciprocal space, which showed that ice grows heterogeneously with a significant population of peaks indicative of truncation rods and crystal defects. Frequent occurrences of the (100) reflection with extended in-planar structure suggested that large planar ice crystals form at the droplet surface, then fracture into smaller domains to accommodate to the curvature of the droplets. Planar faulting due to misaligned domains would explain the increased cubicity close to the droplet surface.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

NASA NTRS1979

Fatigue behavior of SiC reinforced titanium composites

The low cycle axial fatigue properties of 25 and 44 fiber volume percent SiC/Ti(6Al-4V) composites were measured at room temperature and at 650 C. At room temperature, the S-N curves for the composites showed no anticipated improvement over bulk matrix behavior. Although axial and transverse tensile strength results suggest a degradation in SiC fiber strength during composite fabrication, it appears that the poor fatigue life of the composites was caused by a reduced fatigue resistance of the reinforced Ti(6Al-4V) matrix. Microstructural studies indicate that the reduced matrix behavior was due, in part, to the presence of flawed and fractured fibers created near the specimen surfaces by preparation techniques. Another possible contributing factor is the large residual tensile stresses that can exist in fiber-reinforced matrices. These effects, as well as the effects of fatigue testing at high temperature, are discussed.

Bhatt, R. T.↗

NASA NTRS1975

Dynamic SEM wear studies of tungsten carbide cermets

Dynamic friction and wear experiments were conducted in a scanning electron microscope. The wear behavior of pure tungsten carbide and composite with 6 and 15 weight percent cobalt binder was examined. Etching of the binder was done to selectively determine the role of the binder in the wear process. Dynamic experiments were conducted as the WC and bonded WC cermet surfaces were transversed by a 50 micron radiused diamond stylus. These studies show that the predominant wear process in WC is fracture initiated by plastic deformation. The wear of the etched cermets is similar to pure WC. The presence of the cobalt binder reduces both friction and wear. The cementing action of the cobalt reduces granular separation and promotes a dense polished layer because of its low shear strength film-forming properties. The wear debris generated from unetched surface is approximately the same composition as the bulk.

Brainard, W. A.↗

NASA NTRS2020

Stochastic Simulation of Mudcrack Damage Formation in an Environmental Barrier Coating

The FEAMAC/CARES program, which integrates finite element analysis (FEA) with the MAC/GMC (Micromechanics Analysis Code with Generalized Method of Cells) and the CARES/Life (Ceramics Analysis and Reliability Evaluation of Structures / Life Prediction) programs, was used to simulate the formation of mudcracks during the cooling of a multilayered environmental barrier coating (EBC) deposited on a silicon carbide substrate. FEAMAC/CARES combines the MAC/GMC multiscale micromechanics analysis capability (primarily developed for composite materials) with the CARES/Life probabilistic multiaxial failure criteria (developed for brittle ceramic materials) and Abaqus (Dassault Systèmes) FEA. In this report, elastic modulus reduction of randomly damaged finite elements was used to represent discrete cracking events. The use of many small-sized low-aspect-ratio elements enabled the formation of crack boundaries, leading to development of mudcrack-patterned damage. Finite element models of a disk-shaped three-dimensional specimen and a twodimensional model of a through-the-thickness cross section subjected to progressive cooling from 1,300 °C to an ambient temperature of 23 °C were made. Mudcrack damage in the coating resulted from the buildup of residual tensile stresses between the individual material constituents because of thermal expansion mismatches between coating layers and the substrate. A two-parameter Weibull distribution characterized the coating layer stochastic strength response and allowed the effect of the Weibull modulus on the formation of damage and crack segmentation lengths to be studied. The spontaneous initiation of cracking and crack coalescence resulted in progressively smaller mudcrack cells as cooling progressed, consistent with a fractal-behaved fracture pattern. Other failure modes such as delamination, and possibly spallation, could also be reproduced. The physical basis assumed and the heuristic approach employed, which involves a simple stochastic cellular automaton methodology to approximate the crack growth process, are described. The results ultimately show that a selforganizing mudcrack formation can derive from a Weibull distribution that is used to describe the stochastic strength response of the bulk brittle ceramic material layers of an EBC.

Nemeth, Noel N.↗

NASA NTRS1975

Dynamic SEM wear studies of tungsten carbide cermets

Dynamic friction and wear experiments were conducted in a scanning electron microscope. The wear behavior of pure tungsten carbide and composite with 6 and 15 weight percent cobalt binder was examined, and etching of the binder was done to selectively determine the role of the binder in the wear process. Dynamic experiments were conducted as the tungsten carbide (WC) and bonded WC cermet surfaces were transversed by a 50 micron radiused diamond stylus. These studies show that the predominant wear process in WC is fracture initiated by plastic deformation, and the wear of the etched cermets is similar to pure WC. The presence of the cobalt binder reduces both friction and wear. The cementing action of the cobalt reduces granular separation, and promotes a dense polished layer because of its low shear strength film-forming properties. The wear debris generated from unetched surface is approximately the same composition as the bulk.

Brainard, W. A.↗