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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.

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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Multiscale characterization of irradiation behaviour of ion-irradiated SiC/SiC composites

Here, the irradiation tolerance of SiC/SiC composites was studied using 10 MeV Au ion irradiations at 350 °C, for surface doses between 1 and 50 displacements per atom (dpa). Atomic force microscopy and optical profilometry revealed irradiation-induced axial and radial shrinkage of SiC-fibers. At 50 dpa, net fiber shrinkage reached 2.8 ± 0.3%. We conclude that the primary cause of SiC-fiber shrinkage in SiC/SiC composites is the irradiation-induced loss of pre-existing carbon packets, which had occupied 2–3% fiber volume in unirradiated state. A compelling evidence of the carbon packet loss was revealed using a combination of state-of-art conventional transmission electron microscopy (TEM), high resolution TEM, energy-filtered TEM and electron energy loss spectroscopy. Additionally, the carbon packet volume fraction decreased with increasing dose, reaching near-complete loss after 50 dpa. Carbon packet loss was further confirmed using Raman spectroscopy where the carbon D and G peaks disappeared after irradiation. In contrast, irradiation-induced swelling of 1 ± 0.5% was observed in the matrix after 50 dpa. The study also shows that up to 50 dpa, the multilayer pyrolytic-carbon (PyC) interface in the composite is highly irradiation tolerant as it maintained its morphology, graphitic nature and showed no signs of amorphization. Additionally, Raman spectroscopy revealed a saturation of TEM invisible disorder at 1 dpa for both ultra-fine grains of the fiber and the larger SiC-matrix grains. However, TEM visible extended defect formation such as dislocation loops were only detected in the larger matrix grains, thereby revealing a potential role of grain size on defect accumulation in SiC.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Electrochemical aspects of copper atmospheric corrosion in the presence of sodium chloride

Here, this study describes the evolving state of electrolyte and corrosion processes associated with sodium chloride on copper at the initial stage of corrosion and the critical implications of this behavior on controlling kinetics and damage distributions. Sodium chloride droplets were placed on copper in humid conditions and the resulting electrolyte properties, corrosion products and damage were characterized over time using time-lapse imaging, micro Raman spectroscopy, TOF-SIMS and optical profilometry. Within minutes of NaCl droplet placement, NaOH-rich films resultant from oxygen reduction advanced stepwise from the droplets, leaving behind concentric trenching attack patterns suggestive of moving anode-cathode pairs at the alkaline film front. Corrosion attack under these spreading alkaline films was up to 10x greater than under the original NaCl drops. Furthermore, solid Cu 2 Cl(OH) 3 shells formed over the surface of the NaCl drops within hours of exposure. Thermodynamic modeling along with immersed electrochemical experiments in simulated droplet and films electrolytes were used to rationalize this behavior and build a description of the rapidly evolving corroding system.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

A study of adhesive bonding in metal–metal, metal–CFRP, and CFRP–CFRP material combinations under shear deformation: Fracture morphologies and damage mechanisms

Safe design of adhesive joining in multi-materials in engineered structures requires the accumulation of numerous experimental data on the failure behavior of various adhesively-bonded material combinations under different loading conditions. The deep understanding of mechanical performance, fracturing morphologies, and main damage mechanisms is also quintessential for accelerating the development of proper physics-based and multi-scale models for assisting the design. Towards this goal, this work presents a comprehensive characterization of the failure behavior of adhesively-bonded metal–metal, metal–CFRP, and CFRP–CFRP material combinations under global shear deformation via single lap shear testing. Thanks to a synergistic combination of measurement methods by using Digital Imaging Correlation (DIC) and 3D optical profilometry, adhesive features on the adherend after failure were quantified and the main progressive damage mechanisms were identified. The characterization performed in this work provides quantitative data that contributes to a better understanding of shear failure in adhesive bonding across different bi-material combinations. Finally, the obtained results have practical implications, including the potential to enhance adhesive bonding design, identify failure causes in adhesive joints, and develop or validate computational models capable of capturing the observed behavior in various adhesively-bonded materials under global shear deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influence of surface pattern on the biological properties of Ti grade 2

Highlights: • Laser modification causes changes in chemical composition of the surface. • Laser treatment creates roughness in a range from nano- to micrometers. • The surface modification presented results in a multimodal topography. • A hierarchical topography promotes protein adsorption. - Abstract: This paper presents a detailed characterization of Ti surface geometries as produced by non-contact laser functionalization and its impact on the process of protein adsorption. The proposed surface modification is designed for the local treatment of implantable devices with original roughness. In this work, titanium plates were initially modified by the two most common mechano-chemical treatments, shot peening and acid etching. The material under study was next functionalized DLIL (Direct Laser Interference Lithography) in order to obtained two different surface patterns: grooves and islands. The modified surfaces were characterized in terms of their shape, roughness, wettability, surface energy and chemical composition. For this purpose, the following methods were used: scanning electron microscopy, optical profilometry, atomic force microscopy, contact angle measurements, and X-ray photoelectron spectroscopy. Protein adsorption tests were conducted to consider the potential of the proposed methodology in biomedical applications and to compare the influence of the two different surface patterns on the initial state of ossointegration. To this end, XPS and FTIR studies were conducted. The systematic analysis presented will be useful when selecting an appropriate surface geometry for the local surface functionalization of implantable devices.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Surface grain refinement of casting A380 aluminum alloy by ultrasonic-assisted surface mechanical grinding treatment

A novel surface processing technique, ultrasonic-assisted surface mechnical grinding treatment (U-SMGT), was proposed and applied to modify the surface micriostructure of the casting aluminum alloy (A380). Comprehensive post-process chracterization techniques including 3D profilometry, optical microscope, scanning electric microscopy (SEM), and electron backscatter diffraction (EBSD) were carried out to investigate the surface morphology and microstructure of the processed region (PR). It was found that a surface layer of grain refinement with a thickness of about 50 µm was formed. In the as-received base material (BM), large clusters of dendritic eutectic phase with a size of approximately 20 µm were isolated by α-Al matrix. Nano-indentation tests showed that hardness of the eutectic and α-Al in the as-received BM was 2.15 GPa and 1.2 GPa respectively. After U-SMGT, the large dendritic eutectic phase was broken down into much fine particles with an average size of 0.57 µm. These fine particles were uniformly distributed into the α-Al matrix. Nano-indentation measurement exhibited a hardness of 2.27 GPa within the processed region. The overall high hardness in the processed region is a result of the pinning effect of uniformly distributed fine dendrites and grain refinement of Al-matrix.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Scanning angle Raman spectroscopy: A nondestructive method for simultaneously determining mixed polymer fractional composition and film thickness

A scanning angle (SA) Raman spectroscopy method was developed to simultaneously measure the chemical composition and thickness of waveguide mixed polymer films with varying fractional compositions. In order to test the method, six films of polystyrene-block-poly(methyl methacrylate), some mixed with poly(methyl methacrylate) homopolymer (PS-b-PMMA:PMMA), and two films of poly(2-vinylnapthalene)-block-poly(methyl methacrylate) (P2VN-b-PMMA) were prepared. The film thickness ranged from 495 to 971 nm. The chemical composition and thickness of PS-b-PMMA:PMMA films was varied by the addition of the PMMA homopolymer and annealing the films in toluene. SA Raman peak amplitude ratios (1001 cm -1 for PS, 812 cm -1 for PMMA, and 1388 cm -1 for P2VN) were used to calculate the refractive index of the polymer film, an input parameter in calculations of the sum square electric field (SSEF). The film thickness was determined by SSEF models of the experimental Raman amplitudes versus the incident angle of light. The average film thickness determined by the developed SA Raman spectroscopy method was within 5% of the value determined by optical profilometry. In conclusion, SA Raman spectroscopy will be useful for in situ label-free analyses of mixed polymer waveguide films.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Plastic deformation and material transfer on steel gage blocks during low force mechanical probing

Contact probing of gaging surfaces is enabled throughout dimensional metrology. Probe tips such as ruby, sapphire, or diamond are commonly employed as styli for universal length measuring machines (ULMs) and coordinate measuring machines (CMMs) due to the hardness, durability, and wear resistance. Gaging surfaces of gage blocks are precision ground or lapped, with very low surface roughness to enable wringing. Damage or contamination of these surfaces can prevent wringing and lead to measurement error. Experimental investigations using a horizontal ULM and CMM have revealed that even at low force settings (≤0.16 N), probe materials such as ruby and sapphire can cause plastic deformation to hardened carbon chrome steel (such as AISI 52,100) gage block surfaces at the microscale, likely attributed to fretting-associated wear. Under some conditions, permanent transfer of material from the probe stylus to the gaging surface is possible. Results show irreversible changes and damage to gaging surfaces with repeated probe contact on a ULM and CMM. Optical microscopy, optical profilometry, and scanning electron microscopy (SEM) provide a semi-quantitative assessment of microscale plastic deformation and material transfer. X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and Raman techniques validate chemical constituency of reference materials used (gage blocks and probes) and also identify makeup of deposits on gaging surfaces following probe contact.

42 ENGINEERING↗
DOE OSTI2013

Surface Structure Spread Single Crystals (S4C): Preparation and characterization

A set of six spherically curved Cu single crystals referred to as Surface Structure Spread Single Crystals (S{sup 4}Cs) has been prepared in such a way that their exposed surfaces collectively span all possible crystallographic surface orientations that can be cleaved from the face centered cubic Cu lattice. The method for preparing these S{sup 4}Cs and for finding the high symmetry pole point are described. Optical profilometry has been used to determine the true shapes of the S{sup 4}Cs and show that over the majority of the surface, the shape is extremely close to that of a perfect sphere. The local orientations of the surfaces lie within ±1{degree} of the orientation expected on the basis of the spherical shape; their orientation is as good as that of many commercially prepared single crystals. STM imaging has been used to characterize the atomic level structure of the Cu(111)±11{degree}-S{sup 4}C. This has shown that the average step densities and the average step orientations match those expected based on the spherical shape. In other words, although there is some distribution of step-step spacing and step orientations, there is no evidence of large scale reconstruction or faceting. The Cu S{sup 4}Cs have local structures based on the ideal termination of the face centered cubic Cu lattice in the direction of termination. The set of Cu S{sup 4}Cs will serve as the basis for high throughput investigations of structure sensitive surface chemistry on Cu.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Development of ultrananocrystalline diamond (UNCD) coatings for multipurpose mechanical pump seals.

The reliability and performance of silicon carbide (SiC) shaft seals on multipurpose mechanical pumps are improved by applying a protective coating of ultrananocrystalline diamond (UNCD). UNCD exhibits extreme hardness (97 GPa), low friction (0.1 in air) and outstanding chemical resistance. Consequently, the application of UNCD coatings to multipurpose mechanical pump seals can reduce frictional energy losses and eliminate the downtime and hazardous emissions from seal failure and leakage. In this study, UNCD films were prepared by microwave plasma chemical vapor deposition utilizing an argon/methane gas mixture. Prior to coating, the SiC seals were subjected to mechanical polishing using different grades of micron-sized diamond powder to produce different starting surfaces with well-controlled surface roughnesses. Following this roughening process, the seals were seeded by mechanical abrasion with diamond nanopowder, and subsequently coated with UNCD. The coated seals were subjected to dynamic wear testing performed at 3600 RPM and 100 psi for up to 10 days during which the seals were periodically removed and inspected. The UNCD-coated seals were examined using Raman microanalysis, scanning electron microscopy, optical profilometry, and adhesion testing before and after the wear testing. These analyses revealed that delamination of the UNCD films was prevented when the initial SiC seal surface had an initial roughness >0.1 {micro}m. In addition, the UNCD surfaces showed no measurable wear as compared to approximately 0.2 {micro}m of wear for the untreated SiC surfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Electrodeposition and analysis of thick bismuth films

Due to its unique physical and chemical properties, bismuth is an attractive candidate for a wide range of applications such as battery anodes, radiation shielding, and semiconductors, to name a few. This work presents the electrodeposition of mechanically stable and homogenous bismuth films at micron-scale thicknesses. A simple one-step electrodeposition process using either a pulse/reverse or direct current source yielded thick, homogenous, and mechanically stable bismuth films. Morphology, electrochemical behavior, adhesion, and mechanical stability of bismuth coatings plated with varying parameters were characterized via optical profilometry, cyclic voltammetry, electron microscopy, and tribology. Scratch testing on thick electroplated coatings (> 100 µm) revealed similar wear resistance properties between the pulse/reverse plated and direct current electroplated films. This study presents a versatile bismuth electroplating process with the possibility to replace lead in radiation shields with an inexpensive, non-toxic metal, or to make industrially relevant electrocatalytic devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Application of scanning angle Raman spectroscopy for determining the location of buried polymer interfaces with tens of nanometer precision

In this study, near-infrared scanning angle (SA) Raman spectroscopy was utilized to determine the interface location in bilayer films (a stack of two polymer layers) of polystyrene (PS) and polycarbonate (PC). Finite-difference-time-domain (FDTD) calculations of the sum square electric field (SSEF) for films with total bilayer thicknesses of 1200–3600 nm were used to construct models for simultaneously measuring the film thickness and the location of the buried interface between the PS and PC layers. Samples with total thicknesses of 1320, 1890, 2300, and 2750 nm and varying PS/PC interface locations were analyzed using SA Raman spectroscopy. Comparing SA Raman spectroscopy and optical profilometry measurements, the average percent difference in the total bilayer thickness was 2.0% for films less than ~2300 nm thick. The average percent difference in the thickness of the PS layer, which reflects the interface location, was 2.5% when the PS layer was less than ~1800 nm. SA Raman spectroscopy has been shown to be a viable, non-destructive method capable of determining the total bilayer thickness and buried interface location for bilayer samples consisting of thin polymer films with comparable indices of refraction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Multiscale surface roughening of commercial purity titanium during uniaxial tension

The mechanisms of the surface roughening of the titanium specimens during uniaxial tension were demonstrated. By means of optical profilometry and electron backscattered diffraction it was shown that the formation of surface roughening is a multilevel process. The correlation between the density of slip in some grains, and grain rotation, and their displacement towards the free surface was investigated.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Porosity as a function of stoichiometry and implantation temperature in Ge/Si{sub 1−x}Ge{sub x} alloys

The development of porosity in single-crystal germanium and silicon-germanium alloys (c-Si{sub 1−x} Ge{sub x}) of (100) orientation was studied under bombardment with 140 keV Ge{sup −} ions over a wide range of temperatures (−180 to 400 °C) and ion fluences up to 1 × 10{sup 18} ions/cm{sup 2}. The surface swelling and morphology were investigated using multi-characterization techniques including optical profilometry, transmission electron microscopy, and scanning electron microscopy. The initiation of porosity and the evolution of the near-surface microstructure strongly depend on the ion fluence, the irradiation temperature, and the stoichiometry of the substrate. Significant results and new findings include: (i) the fact that, over the entire temperature and stoichiometry range, porosity is only developed once the substrate is rendered amorphous; (ii) with increasing Si content in the alloy, the onset of porosity is pushed to higher fluences; (iii) porosity is observed for Si contents in the alloy up to 23% but not higher under the irradiation conditions used; and (iv) in all cases the initiation of porosity was observed to occur at the surface of the amorphous alloy above a threshold fluence. This last result strongly suggests that the mechanism for initiation of porosity is via preferential vacancy segregation and clustering at the surface of the amorphous alloy. Particularly at elevated temperatures, preferential sputtering of the Si-Ge atomic species in the alloy also plays an important role in developing the surface topography and porosity in alloys. Such effects are discussed along with the implications of our results for mechanisms of porosity in Ge and its alloys.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

The interplay between laser focusing conditions, expansion dynamics, ablation mechanisms, and emission intensity in ultrafast laser-produced plasmas

The interplay between ultrafast laser focusing conditions, emission intensity, expansion dynamics, and ablation mechanisms is critical to the detection of light isotopes relevant to nuclear energy, forensics, and geochemistry applications. Here, we study deuterium (2Hα) emission in plasmas generated from femtosecond laser ablation of a Zircaloy-4 target with a deuterium concentration of ≈37 at. %. Changes in emission intensity, plume morphology, crater dimensions, and surface modifications were investigated for varying focusing lens positions, where the laser was focused behind, at, and in front of the target. Spatially resolved optical emission spectroscopy and spectrally integrated plasma imaging were performed to investigate emission spectral features and plume morphology. Laser ablation crater dimensions and morphology were analyzed via optical profilometry and scanning electron microscopy. The 2Hα emission intensity showed significant reduction at the geometrical focal point or when the focal point is in front of the target. For all laser spot sizes, a two-component plume was observed but with different temporal histories. At the best focal point, the plume was spherical. When the laser was focused behind the target, the plume was elongated and propagated to farther distances than for the best focal position. In contrast, when the laser was focused in front of the target, filaments were generated in the beam path, and filament-plasma coupling occurred. By focusing the laser behind the target, the amount of material removal in the laser ablation process can be significantly reduced while still generating a plasma with a sufficient 2Hα emission signal for analysis.

Kautz, Elizabeth J. (ORCID:0000000263389223)↗
DOE OSTI2022

Impacts of the Additive Manufacturing Process on the Roughness of Engine Scale Vanes and Cooling Channels

Abstract By leveraging the additive manufacturing (AM) platform, development time and costs for turbine component testing can be reduced relative to traditional investment casting. Surface roughness is a key characteristic of the additive manufacturing process that can impact flow, heat transfer, and mechanical integrity of printed components. There are multiple design and build considerations that result in variability in surface roughness, especially when additively fabricating complicated three-dimensional vanes and internal cooling passages. This study characterizes the surface roughness of internal cooling passages, vanes, and flat external surface samples made using additive manufacturing, specifically the direct metal laser sintering process. The samples were manufactured with various wall thicknesses, layer thicknesses, build locations, build directions, and on different AM machines. A combination of computed tomography scanning and optical profilometry was used to evaluate surface roughness levels. The data indicate that the dominant factors in roughness for a given layer thickness are a function of wall thickness, build location, and build direction.

Engineering↗
DOE OSTI2021

Long-Term Effects of Humidity on Stainless Steel Pitting in Sea Salt Exposures

Ground 304 stainless steel (SS) samples were exposed to sea salt particles at 35 °C and two relative humidity (RH) levels for durations ranging from 1 week to 2 years. For all exposure times, pit number density and total pit volume at 40% RH were observed to be considerably greater than those at 76% RH. Statistical analysis of distributions of pit populations for both RH conditions showed that pit number density and total pit volume increased rapidly at first but slowed as exposure time increased. Cross-hatched features were observed in the 40% RH pits while ellipsoidal, faceted pits were observed at 76% RH. Optical profilometry indicated that most pits were not hemispherical. X-ray tomography provided evidence of undercutting and fissures. Piecewise curve fitting modeled the 40% RH data closely, predicting that corrosion damage would eventually plateau. However, a similar treatment of the 76% RH data suggested that corrosion damage would continuously increase, which implied that the piecewise power-law fit was limited in its ability to model atmospheric corrosion generally. Based on these observations, the operative mechanisms determining long-term corrosion behavior were hypothesized to be different depending on the RH of exposure.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Development and calibration of mirrors and gratings for the Soft X-ray materials science beamline at the Linac Coherent Light Source free-electron laser

This article discusses the development and calibration of the x-ray reflective and diffractive elements for the Soft X-ray Materials Science (SXR) beamline of the Linac Coherent Light Source (LCLS) free-electron laser (FEL), designed for operation in the 500 – 2000 eV region. The surface topography of three Si mirror substrates and two Si diffraction grating substrates was examined by atomic force microscopy (AFM) and optical profilometry. The figure of the mirror substrates was also verified via surface slope measurements with a long trace profiler. A boron carbide (B 4 C) coating especially optimized for the LCLS FEL conditions was deposited on all SXR mirrors and gratings. Coating thickness uniformity of 0.14 nm root mean square (rms) across clear apertures extending to 205 mm length was demonstrated for all elements, as required to preserve the coherent wavefront of the LCLS source. The reflective performance of the mirrors and the diffraction efficiency of the gratings were calibrated at beamline 6.3.2 at the Advanced Light Source synchrotron. To verify the integrity of the nanometer-scale grating structure, the grating topography was examined by AFM before and after coating. This is to our knowledge the first time B 4 C-coated diffraction gratings are demonstrated for operation in the soft x-ray region.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Multi-scale Modeling of Plasticity in Tantalum.

In this report, we present a multi-scale computational model to simulate plastic deformation of tantalum and validating experiments. In atomistic/ dislocation level, dislocation kink- pair theory is used to formulate temperature and strain rate dependent constitutive equations. The kink-pair theory is calibrated to available data from single crystal experiments to produce accurate and convenient constitutive laws. The model is then implemented into a BCC crystal plasticity finite element method (CP-FEM) model to predict temperature and strain rate dependent yield stresses of single and polycrystalline tantalum and compared with existing experimental data from the literature. Furthermore, classical continuum constitutive models describing temperature and strain rate dependent flow behaviors are fit to the yield stresses obtained from the CP-FEM polycrystal predictions. The model is then used to conduct hydro- dynamic simulations of Taylor cylinder impact test and compared with experiments. In order to validate the proposed tantalum CP-FEM model with experiments, we introduce a method for quantitative comparison of CP-FEM models with various experimental techniques. To mitigate the effects of unknown subsurface microstructure, tantalum tensile specimens with a pseudo-two-dimensional grain structure and grain sizes on the order of millimeters are used. A technique combining an electron back scatter diffraction (EBSD) and high resolution digital image correlation (HR-DIC) is used to measure the texture and sub-grain strain fields upon uniaxial tensile loading at various applied strains. Deformed specimens are also analyzed with optical profilometry measurements to obtain out-of- plane strain fields. These high resolution measurements are directly compared with large-scale CP-FEM predictions. This computational method directly links fundamental dislocation physics to plastic deformations in the grain-scale and to the engineering-scale applications. Furthermore, direct and quantitative comparisons between experimental measurements and simulation show that the proposed model accurately captures plasticity in deformation of polycrystalline tantalum.

36 MATERIALS SCIENCE↗