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All sourcesNASA NTRSDOE OSTI
NASA NTRS1998

Surface Chemistry, Microstructure, and Tribological Properties of Cubic Boron Nitride Films

This report deals with the surface chemistry, microstructure, bonding state, morphology, and friction and wear properties of cubic boron nitride (c-BN) films that were synthesized by magnetically enhanced plasma ion plating. Several analytical techniques - x-ray photoelectron spectroscopy, transmission electron microscopy and electron diffraction, Fourier transform infrared spectroscopy, atomic force microscopy, and surface profilometry - were used to characterize the films. Sliding friction experiments using a ball-on-disk configuration were conducted for the c-BN films in sliding contact with 440C stainless-steel balls at room temperature in ultrahigh vacuum (pressure, 10(exp -6), in ambient air, and under water lubrication. Results indicate that the boron-to-nitrogen ratio on the surface of the as-deposited c-BN film is greater than 1 and that not all the boron is present as boron nitride but a small percentage is present as an oxide. Both in air and under water lubrication, the c-BN film in sliding contact with steel showed a low wear rate, whereas a high wear rate was observed in vacuum. In air and under water lubrication, c-BN exhibited wear resistance superior to that of amorphous boron nitride, titanium nitride, and titanium carbide.

Watanabe, Shuichi↗
NASA NTRS2014

Assessment of Shape Memory Alloys - From Atoms To Actuators - Via In Situ Neutron Diffraction

As shape memory alloys (SMAs) become an established actuator technology, it is important to identify the fundamental mechanisms responsible for their performance by understanding microstructure performance relationships from processing to final form. Yet, microstructural examination of SMAs at stress and temperature is often a challenge since structural changes occur with stress and temperature and microstructures cannot be preserved through quenching or after stress removal, as would be the case for conventional materials. One solution to this dilemma is in situ neutron diffraction, which has been applied to the investigation of SMAs and has offered a unique approach to reveal the fundamental micromechanics and microstructural aspects of bulk SMAs in a non-destructive setting. Through this technique, it is possible to directly correlate the micromechanical responses (e.g., internal residual stresses, lattice strains), microstructural evolutions (e.g., texture, defects) and phase transformation properties (e.g., phase fractions, kinetics) to the macroscopic actuator behavior. In this work, in situ neutron diffraction was systematically employed to evaluate the deformation and transformation behavior of SMAs under typical actuator conditions. Austenite and martensite phases, yield behavior, variant selection and transformation temperatures were characterized for a polycrystalline NiTi (49.9 at. Ni). As the alloy transforms under thermomechanical loading, the measured textures and lattice plane-level variations were directly related to the cyclic actuation-strain characteristics and the dimensional instability (strain ratcheting) commonly observed in this alloy. The effect of training on the shape memory characteristics of the alloy and the development of two-way shape memory effect (TWSME) were also assessed. The final conversion from a material to a useful actuator, typically termed shape setting, was also investigated in situ during constrained heatingcooling and subsequent shape recovery experiments. Neutron diffraction techniques are also being applied to the investigation of novel high temperature SMAs with the objective of designing alloys with better stability, higher transition temperatures and ultimately superior durability.

Shape Memory Alloys↗
DOE OSTI2024

Impact of Dilute DIO Additive on Local Microstructure of Fluorinated, pNDI‐Based Polymer Solar Cells

The performance of all‐polymer solar cells is often enhanced by incorporating solvent additives during solution processing. Here, in particular, blends based on the model all‐polymer system PBDBT:N2200 have been shown to have increased short‐circuit current and fill factor when processed with dilute diiodooctane (DIO). However, the morphological mechanism that drives the increase in performance is often not well understood due to limitations in common characterization techniques. In this study, it is shown that a combination of X‐ray techniques with cryogenic high‐resolution transmission electron microscopy (HRTEM) analysis can provide a quantitative and spatially resolved picture of polymer chain orientation and alignment in all‐polymer blends. It is found that DIO induces vertical phase separation in PBDBT‐2F:F‐N2200 and increases donor crystallite thickness in the pi‐stacking direction leading to an acceptor‐rich film surface. However, it is also shown that DIO does not disrupt the formation of face‐on donor–acceptor interfaces. These findings suggest that dilute DIO primarily affects crystalline domain formation in single component regions as opposed to mixed regions; thus, dilute DIO can impact vertical charge transport pathways without sacrificing donor–acceptor interfacial connectivity.

Cheng, Christina↗
NASA NTRS1990

Characterization of welded HP 9-4-30 steel for the advanced solid rocket motor

Solid rocket motor case materials must be high-strength, high-toughness, weldable alloys. The Advanced Solid Rocket Motor (ASRM) cases currently being developed will be made from a 9Ni-4Co quench and temper steel called HP 9-4-30. These ultra high-strength steels must be carefully processed to give a very clean material and a fine grained microstructure, which insures excellent ductility and toughness. The HP 9-4-30 steels are vacuum arc remelted and carbon deoxidized to give the cleanliness required. The ASRM case material will be formed into rings and then welded together to form the case segments. Welding is the desired joining technique because it results in a lower weight than other joining techniques. The mechanical and corrosion properties of the weld region material were fully studied.

Watt, George William↗
NASA NTRS2016

InSitu SEM Investigation of Microstructural Damage Evolution and Strain Relaxation in a Melt Infiltrated SiC/SiC Composite

With CMC components poised to complete flight certification in turbine engines on commercial aircraft within the near future, there are many efforts within the aerospace community to model the mechanical and environmental degradation of CMCs. Direct observations of damage evolution are needed to support these modeling efforts and provide quantitative measures of damage parameters used in the various models. This study was performed to characterize the damage evolution during tensile loading of a melt infiltrated (MI) silicon carbide reinforced silicon carbide (SiC/SiC) composite. A SiC/SiC tensile coupon was loaded to a maximum global stress of 30 ksi in a tensile fixture within an SEM while observations were made at 5 ksi increments. Both traditional image analysis and DIC (digital image correlation) were used to quantify damage evolution. With the DIC analysis, microscale damage was observed at the fiber-matrix interfaces at stresses as low as 5 ksi. First matrix cracking took place between 20 and 25 ksi, accompanied by an observable relaxation in strain near matrix cracks. Matrix crack opening measurements at the maximum load ranged from 200 nm to 1.5 m. Crack opening along the fiber-matrix interface was also characterized as a function of load and angular position relative to the loading axis. This characterization was funded by NASA GRC and was performed to support NASA GRC modeling of SiC/SiC environmental degradation

testing↗
DOE OSTI2024

Forming more and sharper sensing protrusions on graphene-based electrodes through annealing

A better understanding of the microstructure, physicochemical properties, and sensing behavior of an electrode is critical in developing quick, high sensitivity, and robust electrochemical sensors. Here, in this study, a single electrode was fabricated with self-prepared graphene ink through a drop-cast process followed with a subsequent annealing treatment. The graphene ink-based electrodes were characterized through AFM, contact angle, FTIR, impedance spectra, Raman, and SEM to understand annealing treatment effects. The dynamic response of the electrode to humidity, and vapors of ethanol, propanol, or acetone was measured using a four-point probe station in a closed chamber. The annealing treatment increased the conductivity of the electrode and improved its sensing performance by forming more and sharper protrusions on the electrode surface. These unique surface protrusions suggest that the annealed graphene ink-based electrodes hold great potential in developing high-performance electrochemical sensors.

42 ENGINEERING↗
DOE OSTI2026

Defect engineering in nickel via electrodeposition following low temperature annealing

Electrodeposited nickel coatings are characterized by high densities of crystalline defects including dislocations, growth twins, and hydrogen bubbles/voids, arising from the non-equilibrium nature of deposition. While these metastable features influence as-deposited properties, their evolution under low temperature annealing remains unexplored. Here, in this study, we demonstrate that low temperature annealing (200 °C) induces significant microstructural rearrangement without grain growth, enabling defect engineering through thermally assisted dislocation motion and twin boundary migration. Notably, we observe faceted twin boundaries and dislocation organization into extended networks, which have been rarely reported under such annealing conditions. These transformations are attributed to hydrogen-assisted defect mobility, facilitated by the release or redistribution of hydrogen trapped during deposition. These structural transformations correlate with a significant enhancement in mechanical properties, including a twofold increase in yield strength and improved ductility. Our findings highlight the role of trapped hydrogen in mediating low-temperature defect mobility and twin boundary evolution, offering a unique pathway for microstructural tuning of metallic coatings through controlled annealing.

36 - MATERIALS SCIENCE↗
DOE OSTI2021

The Fundamental Creep Behavior Model of Gr.91 Alloy by ICME Approach (Final Report)

The current project mainly focused on the fundamental creep cracking mechanism of the Grade 91 system during the operation conditions in the advanced technologies FE power plants and build the link among Composition-Processing Parameters-Phase Stability-Microstructure-Creep Resistance. A model based on computational thermodynamics and diffusion kinetics will be developed to provide guidance on how to improve the creep resistance of the alloy system. The PI mainly investigate the Gr.91 base alloy and weldment with the Integrated Computational Materials Engineering (ICME) approach. The long-term goal of the proposed program is to develop a model for creep and fatigue resistant alloys with different elemental systems, compositions, and processing parameters of weldment and heat-treatment. In addition, new creep and fatigue resistant alloys are to be designed based on the predictions from the model. The computational as well as experimental results include three sections: 1) The compositional optimization and secondary phases evaluation regarding the creep resistance in Grade 91 steel through the CALPHAD approach. In this section, the formation of the critical secondary phases, M23C6, MX and Z-phase were well predicted based on many conditions like the temperature as well as compositions. Meanwhile, the role of different alloying elements was also considered as they will directly affect the formation of the secondary phases mentioned above based on the compositional evolution of the alloying elements. 2) An investigation of Creep Resistance in Grade 91 Steel through Computational Thermodynamics. We systematically considered the evolution of the four critical temperatures, Ac3, Ac1, the threshold of M23C6 and Z-phase, on basis of the computational approach. Meanwhile, the equilibrium cooling as well as Scheil simulations were also considered to perform further predictions based on the different cooling rates. 3) Creep lifetime and microstructural evolution of the Grade 91 steel. In this part, mainly experimental approach was performed on the real creep test from the beginning of the commercial Gr.91 alloys. The alloys were normalized, tempered, welded (Gleeble) and PWHT and finally subjected to the creep lifetime analyses. Finally, all the samples after each process were further characterized based on the OM, XRD and SEM technique to draw final conclusions.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2023

Implementation of Distributed Memory Computing in MOSAIC to Enable Large 3D Simulations of Irradiated Concrete

The concrete biological shield (CBS) of light-water reactors protects workers and the surrounding environment by absorbing neutron and gamma irradiation emitted from the reactor core. The radiation dose increases with the CBS’s operational time and, in the long term, becomes significant enough to raise the question of irradiation effects on concrete—and particularly on the structural integrity of the CBS. Irradiation-induced damage has been identified as one of the main degradation mechanisms in the CBS. Neutron radiation causes the swelling of aggregate-forming minerals at different rates and amplitudes depending on the mineral’s nature. Silicate-bearing minerals such as quartz are particularly sensitive to neutron radiation and experience up to 17.8% volumetric expansion. Aggregates comprise several minerals with different orientations and are, therefore, subject to cracking as a result of mismatch strains. Additionally, the swelling of aggregates creates significant stresses in the surrounding cement paste matrix, which also results in crack formation. In parallel with the collection of characterization and irradiation test data, development of modeling and simulation tools for irradiated concrete is ongoing with the support of the US Department of Energy Office of Nuclear Energy’s Light Water Reactor Sustainability (LWRS) program. This effort resulted in the development and application of the fast-Fourier transform (FFT)–based code Microstructure-Oriented Scientific Analysis of Irradiated Concrete (MOSAIC) at Oak Ridge National Laboratory.

61 RADIATION PROTECTION AND DOSIMETRY↗
NASA NTRS1993

Organometallic chemical vapor deposition and characterization of ZnGe(1-x)Si(x)P2-Ge alloys on GaP substrates

The epitaxial growth of ZnGe(1-x)Si(x)P2-Ge alloys on GaP substrates by open tube organometallic chemical vapor deposition (OMCVD) is reported. The chemical composition of the alloys characterized by energy dispersive X-ray spectroscopy shows that alloys with x up to 0.13 can be deposited on (001) GaP. Epitaxial growth with mirror smooth surface morphology was achieved for x less than or equal to 0.05. Transmission electron microscopy (TEM) micrographs of these alloys show specular epitaxy and the absence of microstructural defects indicating a defect density of less than 10(exp 7) cm(sup -2). Selected area electron diffraction pattern of the alloy shows that the epitaxial layer crystallizes in the chalcopyrite structure with relatively weak superlattice reflections indicating certain degree of randomness in the cation sublattice. Hall measurements show that the alloys are p-type, like the unalloyed films; the carrier concentration, however, dropped about 10 times from 2 x 10(exp 18) to 2 x 10(exp 17) cm(sup -3). Absorption measurements indicate that the band tailing in the absorption spectra of the alloy was shifted about 0.04 eV towards shorter wavelength as compared to the unalloyed material. Diodes fabricated from the n(+)-GaP/p-ZnSiP2-ZnGeP2-Ge heterostructure at x = 0.05 have a reverse break-down voltage of -10.8 V and a reverse saturation current density of approximately 6 x 10(exp -8) A/sq cm.

Xing, G. C.↗
DOE OSTI2024

From irregular to regular eutectic growth in the Al-Al 3 Ni system: In situ observations during directional solidification

Here we investigate the irregular eutectic growth dynamics of the Al-Al 3 Ni alloy, in which one of the solid phases (Al 3 Ni) grows faceted from the liquid. Leveraging in situ optical microscopy and synchrotron transmission x-ray microscopy, we address the question of the degree of coupling between Al and Al 3 Ni at the growth front and that of the shape of the microstructures left behind in the bulk solid during directional solidification. Real-time optical observations bring evidence for a morphological transition from a eutectic-grain dependent, irregular eutectic growth at low solidification velocity V (typically 1 μm s -1 ), to a weakly anisotropic, regular growth at higher V ( reaching 10 μm s -1 ). Unprecedented x-ray nano-imaging of the solid–liquid interface, and 3D characterization of the growth patterns, were made possible by a new DS setup at Brookhaven National Laboratory’s NSLS-II. At low V, the leading tips of partly faceted Al 3 Ni crystals are observed to grow not far ahead of the Al growth front. Correlating in situ images and postmortem 3D tomographic reconstructions reveals that the presence of faceted and non-faceted regions of Al 3 Ni crystals in the solid is a direct consequence of coupling and decoupling during DS, respectively. Upon increasing V, the lead distance of Al 3 Ni vanishes, and the shape of Al 3 Ni ceases to be governed by faceted growth. These observations cast light onto the basic mechanisms (faceted growth, diffusive coupling, and the dynamics of trijunctions) governing a faceted to rod-like transition upon increasing V in the Al 3 Ni system, with broad implications to a large class of irregular eutectics.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Quantifying the Relationship Between Microstructure and Performance in Gadolinium-Doped Ceria Infiltrated Ni/YSZ Symmetric Cells

Infiltration of mixed ionic/electronic conducting (MIEC) nanocatalysts into the anodes of solid oxide fuel cells (SOFCs) allow the hydrogen oxidation reaction (HOR) to occur at double-phase boundaries (DPBs), rather than being confined only to the triple phase boundaries (TPBs). In this research, we use a combination of cross-sectional scanning electron microscopy (SEM), three-dimensional (3-D) reconstruction, and electrochemical methods to characterize both baseline and gadolinium-doped ceria (GDC)-infiltrated symmetric cells, with the goal of establishing a comparison between the density of electrochemically active sites in uninfiltrated and GDC-infiltrated cells. Here, electrochemical impedance spectroscopy (EIS) and distribution of relaxation times (DRT) analysis showed GDC infiltration decreased the overall polarization of the anode by a factor of 8.78 X, and decreased the resistance associated with the reactions at the TPBs/DPBs by a factor of over 21 X. By quantifying expected GDC deposition morphology in the Ni/YSZ anode it is estimated that reactions occur in the baseline cell up to 84 nm from the active TPB lines.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Characterization of Preliminary Powder Production and Consolidation for Advanced LEU Fuel Concepts

A set of novel uranium-based alloys has been proposed for use in advanced LEU fuel systems that utilize powder metallurgical methods for fabrication of the fuel forms. This study seeks to evaluate the effectiveness of current fabrication methods to produce powder of each of the candidate alloys and consolidate composite systems. Powder samples were produced via atomization and analyzed for particle size, shape, and microstructure utilizing sieving methods and scanning electron microscopy (SEM). Preliminary pellet consolidation tests were conducted with the atomized powder using a press and sinter method. The resulting pellets were analyzed via SEM to evaluate the morphology of the composite system. These preliminary tests demonstrate the ability to produce powder but did not yield the desired quality of powder and impacted the ability to fabricate a fully dense pellet. A refined process is under development to produce a higher yield of small (<250 µm) spherical powder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS2011

Fabrication and Characterization of Brazed Joints for SiC-Metallic Systems Utilizing Refractory Metals

Metal to ceramic joining plays a key role for the integration of ceramics into many nuclear, ground and aero based technologies. In order to facilitate these technologies, the active metal brazing of silicon carbide (CVD beta-SiC, 1.1 mm thick, and hot-pressed alpha-SiC, 3 mm thick) to the refractory metals molybdenum and tungsten using active braze alloys was studied. The joint microstructure, composition, and microhardness were evaluated by optical microscopy (OM), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and Knoop hardness testing. The braze alloys, Cusil-ABA, Ticusil and Copper-ABA, all formed sound joints with excellent wetting and chemical bonding with the SiC substrate. Despite the close thermal expansion match between the metal substrates and SiC, hairline cracks formed in alpha-SiC while beta-SiC showed no signs of residual stress cracking. The use of ductile interlayers to reduce the effect from residual stresses was investigated and joints formed with copper as an interlayer produced crack free systems utilizing both CVD and hot-pressed SiC.

Coddington, Bryan↗
DOE OSTI2024

Variation of the Passive Film on Compositionally Concentrated Dual-Phase Al 0.3 Cr 0.5 Fe 2 Mn 0.25 Mo 0.15 Ni 1.5 Ti 0.3 and Implications for Corrosion

The passive film on a dual-phase Al 0.3 Cr 0.5 Fe 2 Mn 0.25 Mo 0.15 Ni 1.5 Ti 0.3 FCC + Heusler (L2 1 ) compositionally concentrated alloy formed during extended exposure to an applied potential in the passive range in dilute chloride solution was characterized. Each phase, with its own distinct composition of passivating elements, formed unique passive films separated by a heterophase interface. High-resolution, surface sensitive characterization enabled chemical analysis of the passive film formed over individual phases. The film formed over the L2 1 phase had a higher concentration of Al, Ni, and Ti, while the film formed over FCC phase was of similar thickness but contained comparatively higher Cr, Fe, and Mo concentrations, consistent with the differences in bulk microstructure composition. The passive film was continuous across phase boundaries and the distribution of passivating elements (Al, Cr, and Ti) indicated both phases were independently passivated. Spatially resolved analysis of the surface chemistry of the dual-phase CCA revealed that the cation with the highest composition in passive film formed on the FCC phase was Cr (52.4 at. pct) and for the L2 1 phase was Ti (53.1 at. pct) despite the bulk concentration of each element being below 20 at. pct in their respective phases. Al, Cr, and Ti were enriched in both phases within the passive film relative to their respective bulk compositions. In parallel studies, single-phase alloys with compositions representative of the FCC and L2 1 phases were synthesized to evaluate the corrosion behavior of each phase in isolation. The corrosion behavior of the dual-phase alloy showed passivity evidenced by a pitting potential of 0.615 V SCE in 0.01 M NaCl. The pitting potential and other electrochemical parameters suggested a combination of behaviors of both single-phase samples, suggesting that the global corrosion behavior may be represented by a composite theory applied to phases, their area fractions, and interphase length. However, the interphase in the dual-phase CCA was a local corrosion initiation site and may limit localized corrosion protectiveness. The alloy design implications for optimization of second phase structure and morphology are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Multiscale investigation of thermomechanical and compositional developments in Ni alloy 718 under laser processing

Laser processing has been widely employed in various applications due to its exceptional spatial resolution. However, the rapid temperature gradients generated in localized areas present significant challenges for experimental characterization using conventional instruments. To characterize Ni alloy 718 during laser processing, we employed in-situ synchrotron X-ray diffraction with a high-speed detector, a method particularly well-suited for probing processes with high temporal and spatial resolution. Through a series of in-situ experiments, we investigated the local variations in the evolution of microstructures and thermomechanical behaviors within a keyhole mode melt pool. The in situ macroscopic thermomechanical behaviors were quantified using an empirical model derived from diffraction patterns, with experimental results showing reasonable agreement with finite element analysis. Various laser parameters were tested to assess their influences on the residual strains in the melt pools. The results revealed that the residual strain in the keyhole mode melt pool is relatively insensitive to variations in the parameters and is smaller than that in the melt pool created under conduction mode laser scanning. Additionally, we analyzed the shapes of individual diffraction spots, providing insights into the plastic behaviors and compositional developments in the resolidified alloy. The analysis confirmed that compositional variations in a dendritic microstructure manifest as asymmetric broadening of the diffraction spots.

Ni alloy 718↗
DOE OSTI2022

Dislocation dynamics in heterogeneous nanostructured materials

Crystalline materials can be strengthened by introducing dissimilar phases that impede dislocation glide. At the same time, the changes in microstructure and chemistry usually make the materials less ductile. One way to circumvent the strength–ductility dilemma is to take advantage of heterogeneous nanophases which simultaneously serve as dislocation barriers and sources. Owing to their superior mechanical properties, heterogeneous nanostructured materials (HNMs) have attracted a lot of attention worldwide. Nevertheless, it has been difficult to characterize dislocation dynamics in HNMs using classical continuum models, mainly due to the challenges in describing the elastic and plastic heterogeneity among the phases. Here, in this work, we advance a phase-field dislocation dynamics (PFDD) model to treat multi-phase materials, consisting of phases differing in composition, structural order, and size in the same system. We then apply the advanced PFDD model to exploring two important but divergent materials design problems in HNMs: dislocation/obstacle interactions and dislocation/interface interactions. Results show that the interactions between a dislocation and distribution of obstacles varying in structure and composition cannot be understood by simply interpolating from their individual interactions with a dislocation. It is also found that materials containing interfaces with nanoscale thicknesses and compositional gradients have a much higher dislocation bypass stress than those with sharp interfaces, providing an explanation for the simultaneous high strength and toughness of thick interface-containing nanolaminates as observed in recent experiments.

36 MATERIALS SCIENCE↗

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