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DOE OSTI2022

Complementarity of neutron, XFEL and synchrotron crystallography for defining the structures of metalloenzymes at room temperature

Room-temperature macromolecular crystallography allows protein structures to be determined under close-to-physiological conditions, permits dynamic freedom in protein motions and enables time-resolved studies. In the case of metalloenzymes that are highly sensitive to radiation damage, such room-temperature experiments can present challenges, including increased rates of X-ray reduction of metal centres and site-specific radiation-damage artefacts, as well as in devising appropriate sample-delivery and data-collection methods. It can also be problematic to compare structures measured using different crystal sizes and light sources. In this study, structures of a multifunctional globin, dehaloperoxidase B (DHP-B), obtained using several methods of room-temperature crystallographic structure determination are described and compared. Here, data were measured from large single crystals and multiple microcrystals using neutrons, X-ray free-electron laser pulses, monochromatic synchrotron radiation and polychromatic (Laue) radiation light sources. These approaches span a range of 18 orders of magnitude in measurement time per diffraction pattern and four orders of magnitude in crystal volume. The first room-temperature neutron structures of DHP-B are also presented, allowing the explicit identification of the hydrogen positions. The neutron data proved to be complementary to the serial femtosecond crystallography data, with both methods providing structures free of the effects of X-ray radiation damage when compared with standard cryo-crystallography. Comparison of these room-temperature methods demonstrated the large differences in sample requirements, data-collection time and the potential for radiation damage between them. With regard to the structure and function of DHP-B, despite the results being partly limited by differences in the underlying structures, new information was gained on the protonation states of active-site residues which may guide future studies of DHP-B.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Development and performance of INCONEL® alloy 740H® seam-welded piping

INCONEL® alloy 740H® is an age-hardenable nickel-based alloy approved for pressure vessels and piping within ASME Section I, VIII, and B31.1. Currently, the code applies a weld strength reduction factor (WSRF) of 0.7 to the allowable stresses for longitudinal seam welds in the time dependent creep regime. In this work, a full-scale seam weld was successfully produced using typical industrial practices. The component was solution heat-treated and aged after fabrication to improve the performance of the weldment. Tensile, bend, impact, and low-cycle fatigue tests showed the component met all the specification requirements and elevated temperature properties were within base metal expectations with failures predominately in the weld metal. Long-term creep tests, including large samples more representative of the entire weldment, were fabricated and tested to times in excess of 10,000 h at multiple temperatures. Analysis of the creep data supports a WSRF of 0.9 for the solution annealed + aged weldments in contrast to the WSRF of 0.7 currently applied to welded + aged weldments. Metallurgical analysis shows that the solution annealing causes recrystallization of the weld metal and reduces the chemical compositional and microstructural gradients in the weldments resulting in acceptable short-term performance. In long-term creep, evidence for coarsened zones in the weldments due to discontinuous coarsening reactions were identified as the mechanism leading to accelerated creep damage formation in the weld metal and sample failure.

14 SOLAR ENERGY↗

DOE OSTI2023

The effect of current and lambda on white-etch-crack failures

White etching cracks (WECs) have been associated with premature failure of wind turbine roller bearings. Various drivers for the generation of WECs have been identified such as loading conditions, slip, steel quality, lubrication, hydrogen embrittlement, corrosion fatigue cracking, and stray electrical currents passing through the surface. Here, in this work, a benchtop test rig utilizing a three-ring-on-roller test configuration was used to investigate the effect of electrical current and operation in different lubricating regimes, defined by lambda (λ), on high-quality bearing steel samples tested in a commercially available power transmission EP gear lubricant. It was observed that there is an inverse correlation between the magnitude of electric current applied to the ring/ roller system and time-to-failure. Higher current magnitudes lead to shorter time-to-failure than lower current magnitudes, with macropitting as the main failure mode. Sub-surface investigation revealed the presence of WECs in all cases. For the same current magnitude, tests conducted in boundary and mixed lubrication regimes showed that time-to-failure increased as lambda increased, and the tests resulted in WEC related macropits, whereas tests conducted in near-hydrodynamic regime resulted in surface damage with no macropit. It was also noted that a shift toward near-hydrodynamic lubrication resulted in a distinct surface distress on the roller surface. Furthermore, there seems to be a transition in the mixed regime during which the surface distress occurred. The damage on the surface of the test samples resembled non-spatially, periodic, groove-like corrugations and, in some cases, crater-like depressions. Sub-surface imaging, performed by sequential sectioning, revealed the presence of WECs in all cases, and broad, branching cracks that were more prevalent under the more severe boundary conditions.

17 WIND ENERGY↗

NASA NTRS2005

Thermographic Characterization of Impact Damage in SiC/SiC Composite Materials

SiC/SiC composite materials targeted as turbine components for next-generation aero-engines are being investigated at NASA Glenn Research Center. In order to examine damage mechanisms in these materials, SiC/SiC coupons were impacted with 1.59 mm diameter steel spheres at increasing velocities from 115 m/s to 400 m/s. Pulsed thermography, a nondestructive evaluation technique that monitors the thermal response of a sample over time, was utilized to characterize the impact damage. A thermal standard of similar material was fabricated to aid in the interpretation of the thermographic data and to provide information regarding thermography system detection capabilities in 2.4 mm thick SiC/SiC composite materials. Flat bottom holes at various depths with aspect ratios greater than 2.5 were detectable in the thermal images. In addition, the edges of holes at depths of 1.93 mm into the sample were not as resolvable as flat bottom holes closer to the surface. Finally, cooling behavior was characterized in SiC/SiC materials and used to determine impact damage depth within an 8.5% error of a known depth.

Fox, Dennis S.↗

DOE OSTI2020

Multi-scale experimental study of creep-fatigue failure initiation in a 709 Stainless Steel alloy using high resolution digital image correlation. Final report

This report discusses the efforts made towards the multi-scale study of the creep-fatigue response of stainless steel 709. Multiple experimental techniques, including digital image correlation (DIC) and electron backscatter diffraction (EBSD), were used in assessing the evolution of damage accumulation during fatigue, creep-fatigue, and thermomechanical fatigue of alloy 709. The role of microstructural features, hold times, temperature, and loading profiles were quantified and the interchangeability of temperature and time was investigated. Finally, a thermomechanical fatigue model was shown to predict well the failure of samples with varying loading profiles. Results indicate that strain accumulation in 709 steel happens primarily near grain boundaries (GBs) with the strains around GBs being inversely proportional to their measured residual burgers vector. Furthermore, hot-spots for strain accumulation were shown to be the locations of eventual microcrack nucleation. The introduction of hold times to the periodic loading cycle increases the damage accumulation rate and thus shortens the fatigue life of samples–this was true for both room temperature and high temperature. Thermomechanical cycling was shown to have little effect on the end life of samples, with the damage accumulation rate for in-phase and out-of-phase cycling being similar to isothermal fatigue. The interchangeability of time and temperature was shown to be possible within the studied load, time, and temperature ranges, since deformation mechanisms driving strain accumulation did not change with temperature (up to 650°C). The Neu-Sehitoglu thermomechanical fatigue model, with constants obtained from the literature and in part from our experimental results, was applied to predict failure of isothermal creep-fatigue samples. The main objectives of this work were to:(a) Perform high-resolution digital image correlation measurements (HiDIC) for alloy 709; (b) Quantify and assess damage accumulation at the microstructure under fatigue, TMF, and creep-fatigue conditions of 709; (c) Study of the role of hold times, i.e., adding a creep component, to: Room temperature cycling, High temperature cycling, Failure; (d) Study the mechanisms of thermomechanical fatigue in this alloy; (e) Investigate the existence of a time-temperature interchangeability criterion to aid in accelerated creep-fatigue testing; (f) Establish the validity of a combined creep-fatigue model for life prediction for 709. This report is structured with each subsequent section detailing the efforts, results, and conclusions related to each of the objectives described, mostly in chronological order.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Electron energy loss spectroscopy study of ceria sinters and nanoparticles irradiated with swift heavy ions

The electronic energy loss spectra of ceria (CeO 2 ) irradiated with swift heavy ions (27 MeV Xe and 946 MeV Au) in the electronic slowing down regime were measured for bulk sintered samples and nanoparticles by using a double Cs-corrected transmission electron microscope. The low-loss region as well as the core-loss region, including the oxygen K-edge and cerium M 4, 5 white lines, were recorded. No strong lattice disorder was found in the low-loss peaks for both types of samples showing the same bulk oxygen plasmon loss peak at about 15 eV. However, there is a clear evidence of cerium reduction to the trivalent oxidation state after irradiation for the sintered samples as shown by the K-edge shape of oxygen and decrease of the Ce M 4 /M 5 intensity ratio. A similar change of the M 4 /M 5 intensity ratio was observed for the irradiated nanoparticles with respect to the virgin sample owing to the high energy input inside the nanograin. The effect of radiation damage on electron energy loss spectroscopy data is analyzed for both types of samples and irradiation conditions.

Crystallographic defects↗

NASA NTRS2011

Material Characterization and Geometric Segmentation of a Composite Structure Using Microfocus X-Ray Computed Tomography Image-Based Finite Element Modeling

This study utilizes microfocus x-ray computed tomography (CT) slice sets to model and characterize the damage locations and sizes in thermal protection system materials that underwent impact testing. ScanIP/FE software is used to visualize and process the slice sets, followed by mesh generation on the segmented volumetric rendering. Then, the local stress fields around several of the damaged regions are calculated for realistic mission profiles that subject the sample to extreme temperature and other severe environmental conditions. The resulting stress fields are used to quantify damage severity and make an assessment as to whether damage that did not penetrate to the base material can still result in catastrophic failure of the structure. It is expected that this study will demonstrate that finite element modeling based on an accurate three-dimensional rendered model from a series of CT slices is an essential tool to quantify the internal macroscopic defects and damage of a complex system made out of thermal protection material. Results obtained showing details of segmented images; three-dimensional volume-rendered models, finite element meshes generated, and the resulting thermomechanical stress state due to impact loading for the material are presented and discussed. Further, this study is conducted to exhibit certain high-caliber capabilities that the nondestructive evaluation (NDE) group at NASA Glenn Research Center can offer to assist in assessing the structural durability of such highly specialized materials so improvements in their performance and capacities to handle harsh operating conditions can be made.

Abdul-Aziz, Ali↗

NASA NTRS1989

Electron Spin Resonance (ESR) studies of returned comet nucleus samples

The most important objective of the Comet Nucleus Sample Returm Mission is to return samples which could reflect formation conditions and evolutionary processes in the early solar nebula. It is expected that the returned samples will consist of fine-grained silicate materials mixed with ices composed of simple molecules such as H2O, NH3, CH4 as well as organics and/or more complex compounds. Because of the exposure to ionizing radiation from cosmic-ray, gamma-ray, and solar wind protons at low temperature, free radicals are expected to be formed and trapped in the solid ice matrices. The kind of trapped radical species together with their concentration and thermal stability can be used as a dosimeter as well as a geothermometer to determine thermal and radiation histories as well as outgassing and other possible alternation effects since the nucleus material was formed. Since free radicals that are known to contain unpaired electrons are all paramagnetic in nature, they can be readily detected and characterized in their native form by the Electron Spin Resonance (ESR) method. In fact, ESR has been shown to be a non-destructive, highly sensitive tool for the detection and characterization of paramagnetic, ferromagnetic, and radiation damage centers in terrestrial and extraterrestrial geological samples. The potential use of ESR as an effective method in the study of returned comet nucleus samples, in particular, in the analysis of fine-grained solid state icy samples is discussed.

Tsay, Fun-Dow↗

NASA NTRS2014

Effects of Low Earth Orbit on Docking Seal Materials

Spacecraft docking seals are typically made of silicone elastomers. When such seals are exposed to low Earth orbit (LEO) conditions, they can suffer damage from ultraviolet (UV) radiation and atomic oxygen (AO, or monoatomic oxygen, the predominant oxygen species in LEO). An experiment flew on the International Space Station (ISS) to measure the effects of LEO on seal materials S0383-70 and ELA-SA-401 and various mating counterface materials which included anodized aluminum. Samples flown in different orientations received different amounts of UV and AO. The hypotheses were that most of the damage would be from UV, and 10 days or more of exposure in LEO would badly damage the seals. Eighteen seals were exposed for 543 days in ram (windward), zenith (away from Earth), or wake (leeward) orientations, and 15 control samples (not flown) provided undamaged baseline leakage. To determine post-flight leak rates, each of the 33 seals were placed in an O-ring groove of a leak test fixture and pressure tested over time. Resistance temperature detectors (RTDs), pressure transducers, and LabVIEW (National Instruments) programs were used to measure and analyze the temperature and pressure and calculate leakage. Average leakage of control samples was 2.6 x 10(exp -7) lbs/day. LEO exposure did not considerably damage ELA-SA-401. The S0383-70 flight samples leaked at least 10 times more than ELA-SA-401 in all cases except one, demonstrating that ELA-SA-401 may be a more suitable sealing material in LEO. AO caused greater damage than UV; samples in ram orientation (receiving an AO fluence of 4.3 x 10(exp 21) atoms/(sq cm) and in wake (2.9x 10(exp 20) atoms/(sq cm)) leaked more than those in zenith orientation (1.58 x 10(exp 20) atoms/(sq cm)), whereas variations in UV exposure did not seem to affect the samples. Exposure to LEO did less damage to the seals than hypothesized, and the data did not support the conjecture that UV causes more damage than AO.

Leakage↗

NASA NTRS1993

Degradation of optical components in a space environment

Phillips Laboratory's Long Duration Exposure Facility (LDEF) optical experiment is designed to determine the adverse effects of the natural space environment on laser optical component and coating materials. The experiment consists of 10 sample sets, each containing six different material samples. The materials were chosen because of their common use in laser optical components. Sample characterization is divided into three phases. Phase 1 testing is limited to visual and optical performance evaluation. Phase 2 tests investigate the fundamental causes of the performance degradation quantified in Phase 1. During Phase 3, selected samples will be cleaned and some Phase 1 measurements repeated to determine if acceptable optical performance can be restored, and laser damage testing will be performed on a small number of samples. Performance deteriorations will be correlated to exposure duration, sample location on the LDEF, atomic oxygen levels, and other space environment conditions. Preliminary results obtained on the optical samples are discussed.

Dehainaut, Linda L.↗

DOE OSTI2021

4D-STEM of Beam-Sensitive Materials

We report that a scanning electron nanobeam diffraction, or 4D-STEM (four-dimensional scanning transmission electron microscopy), is a flexible and powerful approach to elucidate structure from "soft" materials that are challenging to image in the transmission electron microscope because their structure is easily damaged by the electron beam. In a 4D-STEM experiment, a converged electron beam is scanned across the sample, and a pixelated camera records a diffraction pattern at each scan position. This four-dimensional data set can be mined for various analyses, producing maps of local crystal orientation, structural distortions, crystallinity, or different structural classes. Holding the sample at cryogenic temperatures minimizes diffusion of radicals and the resulting damage and disorder caused by the electron beam. The total fluence of incident electrons can easily be controlled during 4D-STEM experiments by careful use of the beam blanker, steering of the localized electron dose, and by minimizing the fluence in the convergent beam thus minimizing beam damage. This technique can be applied to both organic and inorganic materials that are known to be beam-sensitive; they can be highly crystalline, semicrystalline, mixed phase, or amorphous. One common example is the case for many organic materials that have a π-π stacking of polymer chains or rings on the order of 3.4-4.2 Å separation. If these chains or rings are aligned in some regions, they will produce distinct diffraction spots (as would other crystalline spacings in this range), though they may be weak or diffuse for disordered or weakly scattering materials. We can reconstruct the orientation of the π-π stacking, the degree of π-π stacking in the sample, and the domain size of the aligned regions. This Account summarizes illumination conditions and experimental parameters for 4D-STEM experiments with the goal of producing images of structural features for materials that are beam-sensitive. We will discuss experimental parameters including sample cooling, probe size and shape, fluence, and cameras. 4D-STEM has been applied to a variety of materials, not only as an advanced technique for model systems, but as a technique for the beginning microscopist to answer materials science questions. It is noteworthy that the experimental data acquisition does not require an aberration-corrected TEM but can be produced on a variety of instruments with the right attention to experimental parameters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1986

Effects of temperature and hold times on low cycle fatigue of Astroloy

Low cycle fatigue (LCF) and creep-fatigue-environment interactions of HIP Astroloy were studied at 650 C and 725 C. The results showed that the model proposed by Kaisand and Mowbray (1979) was successful in predicting the magnitude and trend of the fatigue crack growth rate from LCF data. Raising the temperature from 650 C to 725 C did not change the fracture mode, while employing tensile hold caused a change in fracture mode and was more damaging than raising the temperature by 75 C. All samples displayed multiple fracture origins, which is initiated transgranularly in continuous cycling tests and intergranularly in hold time tests. An examination of the secondary crack showed no apparent creep damage. Oxidation in high purity argon appeared to be the major factor in LCF life degradation due to hold time.

Choe, S. J.↗

DOE OSTI2020

Understanding the Structure and Dynamics of Complex Biomembrane Interactions by Neutron Scattering Techniques

The membrane is one of the key structural materials of biology at the cellular level. Composed predominantly of a bilayer of lipids with embedded and bound proteins, it defines the boundaries of the cell and many organelles essential to life and therefore is involved in almost all biological processes. Membrane-specific interactions, such as drug binding to a membrane receptor or the interactions of an antimicrobial compound with the lipid matrix of a pathogen membrane, are of interest across the scientific disciplines. Herein we present a review, aimed at nonexperts, of the major neutron scattering techniques used in membrane studies: small-angle neutron scattering, neutron membrane diffraction, neutron reflectometry, quasielastic neutron scattering, and neutron spin echo. Neutron scattering techniques are well suited to studying biological membranes. The nondestructive nature of cold neutrons means that samples can be measured for long periods without fear of beam damage from ultraviolet, electron, or X-ray radiation, and neutron beams are highly penetrating, thus offering flexibility in samples and sample environments. Most important is the strong difference in neutron scattering lengths between the two most abundant forms of hydrogen, protium and deuterium. Changing the relative amounts of protium/deuterium in a sample allows the production of a series of neutron scattering data sets, enabling the observation of differing components within complex membrane architectures. This approach can be as simple as using the naturally occurring neutron contrast between different biomolecules to study components in a complex by changing the solution H 2 O/D 2 O ratio or as complex as selectively labeling individual components with hydrogen isotopes. This review presents an overview of each experimental technique with the neutron instrument configuration, related sample preparation and sample environment, and data analysis, highlighted by a special emphasis on using prominent neutron contrast to understand structure and dynamics. This review gives researchers a practical introduction to the often enigmatic suite of neutron beamlines, thereby lowering the barrier to taking advantage of these large-facility techniques to achieve new understandings of membranes and their interactions with other molecules.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2004

Damage Detection in Rotorcraft Composite Structures Using Thermography and Laser-Based Ultrasound

New rotorcraft structural composite designs incorporate lower structural weight, reduced manufacturing complexity, and improved threat protection. These new structural concepts require nondestructive evaluation inspection technologies that can potentially be field-portable and able to inspect complex geometries for damage or structural defects. Two candidate technologies were considered: Thermography and Laser-Based Ultrasound (Laser UT). Thermography and Laser UT have the advantage of being non-contact inspection methods, with Thermography being a full-field imaging method and Laser UT a point scanning technique. These techniques were used to inspect composite samples that contained both embedded flaws and impact damage of various size and shape. Results showed that the inspection techniques were able to detect both embedded and impact damage with varying degrees of success.

Anastasi, Robert F.↗

DOE OSTI2025

What more can be done with XPS? Highly informative but underused approaches to XPS data collection and analysis

Because of the importance of surfaces and interfaces in many scientific and technological areas, the use of x-ray photoelectron spectroscopy (XPS) has been growing exponentially. Although XPS is being used to obtain useful information about the surface composition of samples, much more information about materials and their properties can be extracted from XPS data than commonly obtained. This paper describes some of the areas where alternative analysis methods or experimental design can obtain information about the near-surface region of a sample, often information not available in other ways. Experienced XPS analysts are familiar with many of these methods, but they may not be known to new or casual XPS users, and sometimes, they have not been used because of an inappropriately assumed complexity. The information available includes optical, electronic, and electrical properties; nanostructure; expanded chemical information; and enhanced analysis of biological materials and solid/liquid interfaces. Many of these analyses can be conducted on standard laboratory XPS systems, with either no or relatively minor system alterations. Topics discussed include (1) considerations beyond the “traditional” uniform surface layer composition calculation, (2) using the Auger parameter to determine a sample property, (3) use of the D parameter to identify sp 2 and sp 3 carbon information, (4) information from the XPS valence band, (5) using cryocooling to expand range of samples that can be analyzed and minimize damage, and (6) using electrical potential effects on XPS signals to extract chemically resolved electrical measurements including band alignment and electrical property information.

Baer, Donald R. [Pacific Northwest National Labora↗

NASA NTRS1973

Test of LOX compatibility for asphalt and concrete runway materials

A literature survey and a telephone canvass of producers and users of LOX is reported which yielded one report of an accident resulting from a LOX spill on asphalt, one discussion of hazardous conditions, and an unreferenced mention of an incident. Laboratory tests using standard LOX impact apparatus yielded reactions with both old and new alphalt, but none with concrete. In the final test, using a larger sample of asphalt, the reaction caused extensive damage to equipment. Initial field experiments using 2-meter square asphalt slabs covered with LOX, conducted during rainy weather, achieved no reaction with plummets, and limited reaction with a blasting cap as a reaction initiator. In a final plummet-initiated test on a dry slab, a violent reaction, which appeared to have propagated over the entire slab surface, destroyed the plummet fixture and threw fragments as far as 48 meters.

Moyers, C. V.↗

NASA NTRS2003

Neural-Net Based Optical NDE Method for Structural Health Monitoring

This paper answers some performance and calibration questions about a non-destructive-evaluation (NDE) procedure that uses artificial neural networks to detect structural damage or other changes from sub-sampled characteristic patterns. The method shows increasing sensitivity as the number of sub-samples increases from 108 to 6912. The sensitivity of this robust NDE method is not affected by noisy excitations of the first vibration mode. A calibration procedure is proposed and demonstrated where the output of a trained net can be correlated with the outputs of the point sensors used for vibration testing. The calibration procedure is based on controlled changes of fastener torques. A heterodyne interferometer is used as a displacement sensor for a demonstration of the challenges to be handled in using standard point sensors for calibration.

Decker, Arthur J.↗

NASA NTRS2003

Sensitivity and Calibration of Non-Destructive Evaluation Method That Uses Neural-Net Processing of Characteristic Fringe Patterns

Decker, Arthur J.↗