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DOE OSTI2023

Aligned Conjugated Polymer Nanofiber Networks in an Elastomer Matrix for High-Performance Printed Stretchable Electronics

Conjugated polymer films are promising in wearable X-ray detection. However, achieving optimal film microstructure possessing good electrical and detection performance under large deformation via scalable printing remains challenging. Herein, we report bar-coated high-performance stretchable films based on a conjugated polymer P(TDPP-Se) and elastomer SEBS blend by optimizing the solution-processing conditions. The moderate preaggregation in solution and prolonged growth dynamics from a solvent mixture with limited dissolving capacity is critical to forming aligned P(TDPP-Se) chains/crystalline nanofibers in the SEBS phase with enhanced π–π stacking for charge transport and stress dissipation. The film shows a large elongation at break of >400% and high mobilities of 5.29 cm 2 V –1 s –1 at 0% strain and 1.66 cm 2 V –1 s –1 over 500 stretch–release cycles at 50% strain, enabling good X-ray imaging with a high sensitivity of 1501.52 μC Gy air –1 cm –2 . Finally, our work provides a morphology control strategy toward high-performance conjugated polymer film-based stretchable electronics.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Pattern formation on free surfaces via plastic buckling and periodic folding

Spontaneous formation of surface patterns such as folds and creases is widely observed in engineered systems, such as thin films and machined surfaces, as well as in natural systems such as floral petals and leaves. A recognized route for their formation is via surface elastic instabilities. Here we demonstrate an alternate route for their formation —plastic buckling and folding—that occurs when ductile materials are subject to large-strain (>1) deformation. Using in situ imaging of simple-shear deformation of polypropylene, we delineate the mechanics underlying formation of folds and the resulting surface morphology. Here, the fold pattern shows a single wavelength that scales linearly with the size of the plastic zone. An analytical model predicts onset of the plastic buckling instability and characteristics of the folds. Besides obvious applications for controllably generating surface features over large areas, our results suggest a contributing mechanism for origin of surface roughness in solids.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2024

Enabling Digital Image Correlation for Deployment in the Hot Fuels Examination Facility

Digital image correlation (DIC) is a non-contact image-based technique for displacement and strain measurement. It is also a full-field method that can provide excellent spatial resolution. DIC has been widely used for measurements in many styles of mechanical tests and is desirable in part because of this flexibility to measure nearly any material across a range of time and length scales. Its ability to measure localized strain for tests and in environments not accessible to other strain measurement techniques makes it an ideal option for several mechanical test cases that exist in hot cell facilities such as the Hot Fuel Examination Facility (HFEF) at the Idaho National Laboratory (INL). However, DIC has not been demonstrated at HFEF, and several barriers to implementation in the hot cell environment exist. This report outlines the possible paths for deploying DIC at HFEF, weighing the technical advantages and risks with each path. It also discusses the steps which must be taken to add this capability to the suite of post-irradiation examination (PIE) techniques available at HFEF. Finally, it concludes with recommendations for the best method to perform DIC at the facility.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Analysis of Deformation and Fracture Mechanisms in the Harvested High-Dose Baffle-Former Bolt with Stress-Corrosion Cracks Formed While in Service

This report presents the results of advanced mechanical testing conducted on miniature tensile specimens excised from an irradiated baffle-former bolt, a commercial pressurized water reactor component. The specimens were extracted from the midsection of the bolt shank, where the estimated damage dose reached 23 displacements per atom. The mechanical testing included the following tests: (1) conventional tensile testing at room temperature, augmented by digital image correlation (DIC) to enable noncontact strain measurements, and (2) in situ tensile testing within a scanning electron microscopy (SEM) instrument equipped with energy-dispersive x-ray spectroscopy (EDS) and electron backscatter diffraction (EBSD) detectors to evaluate active deformation and fracture mechanisms. Additionally, SEM fractographic analysis revealed alterations in the fracture mechanism from a predominantly ductile fracture in nonirradiated steel to a mixed fracture mode (still dominating ductile and minor cleavage spots) in irradiated specimens derived from the baffle bolts. The findings indicate a complex strain localization behavior for in-service irradiated steel specimens. Beyond conventional necking at the macro scale and defect-free channel formation at the micro scale, DIC results identified the presence of deformation bands approximately 100 μm in width. These bands consist of chains of grains exhibiting elevated local strain levels and may be considered an intermediate or mesoscale level of strain localization. These bands become discernible near the yield stress as localized hot spots, areas of elevated strain, persisting throughout most of the experiment. The formation of mesoscale deformation bands as a strain localization mechanism may exacerbate the defect-free channel formation in irradiated materials, further promoting irradiation-assisted stress corrosion crack initiation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1990

Image correlation nondestructive evaluation of impact damage in a glass fiber composite

Presented in viewgraph format, digital image correlation, damage in fibrous composites, and damaged coupons (cross-ply scotchply GI-Ep laminate) are outlined. It was concluded that the image correlation accuracy was 0.03 percent; strains can be processed through Tsai-Hill failure criteria to qualify the damage; the statistical data base must be generated to evaluate certainty of the damage estimate; size effects need consideration; and better numerical techniques are needed.

Russell, Samuel S.↗

NASA NTRS2002

Evaluation of Mechanical Modal Characteristics Using Optical Techniques

In this paper the sensitivity of embedded fiber optic sensors to changes in modal characteristics of plates is discussed. In order to determine the feasibility of embedded fiber Bragg gratings for the detection of modal shapes and modal frequencies, a comparison of holographically imaged modes and the detected dynamic strain from embedded fiber optic Bragg gratings is made. Time averaged optical holography is used for the detection of mechanical defects, or damage, in various aerospace components. The damage is detected by measuring an alteration in structural dynamics, which is visually apparent when using time-averaged holography. These shifts in the mode shapes, both in frequency of the resonance and spatial location of vibration nodes, are caused by changes in parameters that affect the structure's mechanical impedance, such as stiffness, mass and damping, resulting from cracks or holes. It is anticipated that embedded fiber optic sensor arrays may also be able to detect component damage by sensing these changes in modal characteristics. This work is designed to give an initial indication to the feasibility of damage detection through the monitoring of modal frequencies and mode shapes with fiber optic sensors.

Lekki, John↗

NASA NTRSDate not supplied

Testing of a Multi-Stringer Post-Buckled Panel with Incremental Damage Detection

A multi-stringer panel was designed and tested to produce a failure mode of skin-stiffener delamination due to compression loading of a post-buckled skin to support the validation of high-fidelity progressive damage failure analysis modeling. The test procedure included multiple methods of data acquisition ranging from multiple strain gages, front and back digital image correlation, passive thermography, acoustic emission, and ultrasonic inspection to capture key events and damage progression prior to catastrophic failure. Detailed data showing the initial stiffness, onset of skin buckling, buckled mode shape, damage initiation load, damage propagation morphology, and peak load was captured. Two panel configurations were tested. The first had a Teflon insert placed in the interface between the skin and the stiffener flanges adjacent to the center skin bay. The second was subjected to impact damage to the skin-stiffener flange. In each case, continuously-loaded-to-failure tests were conducted first with passive thermography being used exclusively to determine key damage events. Then, incrementally loaded tests were completed where ultrasonic inspections were conducted between each increment. The amount of load applied between each increment was determined based on the in-situ damage detection provided by the passive thermography system. The results of the testing showed a complex delamination growth pattern which migrated between ply interfaces through matrix splits in the upper skin ply of the panel. The result of the testing produced very detailed data which will prove to be useful for validation of delamination growth and migration predictions from progressive damage failure analysis methods.

Jason Action↗

NASA NTRSDate not supplied

Advances in Integrally Formed Metallic Structures

NASA Langley Research Center (LaRC) is applying flow forming technology to aerospace aluminum alloys for the manufacture of integrally stiffened cylinders that meet aircraft fuselage or launch vehicle specifications. High-strength 2xxx series alloys, in various temper/product form conditions, are being compared with medium-strength, very formable AA 6061 as the benchmark. Screening of candidate materials traditionally relies on empirical forming trials, but more recently on metrics derived from constant nominal strain rate tensile testing. In this work, the established hierarchy of formability metrics is adopted as the baseline; tensile area reduction, work hardening exponent, and modulus of resilience. The suite of metrics can be expanded based on phenomenological and mechanistic considerations of plastic flow instabilities to incorporate anisotropy ratio, rate of work hardening, and dynamic strain aging effects. Separate research thrusts at LaRC are aimed at formulating a protocol for scalable production of fully formed, defect-free components: 1) quantifying the extended set of formability metrics from constant and jump strain rate tensile tests with digital image correlation (DIC); 2) using statistically designed experiments on a vertical spin/flow forming facility (WF VUD-600®) to isolate the effect of convenient process variables, such as axial feed rate and thickness reduction; and 3) predicting the effect of feed ratio (roller translation relative to mandrel rotation speeds) on material response via process modeling using the DEFORM® simulation software. Current results will be discussed in terms of correlating intrinsic material properties with the bulk workability characteristics to successfully fabricate cylinders with complex cross-sections.

Aluminum↗

DOE OSTI2020

Imaging phonon dynamics with ultrafast electron microscopy: Kinematical and dynamical simulations

Ultrafast x-ray and electron scattering techniques have proven to be useful for probing the transient elastic lattice deformations associated with photoexcited coherent acoustic phonons. Indeed, femtosecond electron imaging using an ultrafast electron microscope (UEM) has been used to directly image the influence of nanoscale structural and morphological discontinuities on the emergence, propagation, dispersion, and decay behaviors in a variety of materials. Here, we describe our progress toward the development of methods ultimately aimed at quantifying acoustic-phonon properties from real-space UEM images via conventional image simulation methods extended to the associated strain-wave lattice deformation symmetries and extents. Using a model system consisting of pristine single-crystal Ge and a single, symmetric Lamb-type guided-wave mode, we calculate the transient strain profiles excited in a wedge specimen and then apply both kinematical- and dynamical-scattering methods to simulate the resulting UEM bright-field images. While measurable contrast strengths arising from the phonon wavetrains are found for optimally oriented specimens using both approaches, incorporation of dynamical scattering effects via a multi-slice method returns better qualitative agreement with experimental observations. Contrast strengths arising solely from phonon-induced local lattice deformations are increased by nearly an order of magnitude when incorporating multiple electron scattering effects. We also explicitly demonstrate the effects of changes in global specimen orientation on the observed contrast strength, and we discuss the implications for increasing the sophistication of the model with respect to quantification of phonon properties from UEM images.

36 MATERIALS SCIENCE↗

DOE OSTI2024

High-throughput chemical imaging for optimizing biofuel synthesis using synthetic biology (Final Technical Report)

Fatty acids can be produced biosynthetically in microbes and these compounds can serve as precursors to biodiesels and other high value oleochemicals. However, progress on engineering fatty acid biosynthesis, and biofuel synthesis more generally, has been hindered by current quantification methods that are either indirect or not amenable to high-throughput or single-cell resolution screening. In this project, we assembled an interdisciplinary team with complimentary expertise in synthetic biology and microscopy, metabolic engineering, and chemical imaging to address these challenges. We used chemical imaging to directly measure lipid biosynthesis in Escherichia coli engineered to produce fatty acids, obtaining detailed single-cell resolution measurements. We deployed stimulated Raman scattering (SRS) microscopy in concert with multiplexed genome engineering and gene circuit design strategies from synthetic biology to optimize production of fatty acids. These results provided novel insight into cell-to-cell heterogeneity present in biofuel production strains. In addition, we introduced new chemical imaging methods which are label-free and do not require fluorescent reporters. These efforts were complemented by other studied developing foundational tools for regulation and control, which offer excellent potential for advancing researchers’ ability to rapidly design, build, and test strains for enhanced biofuel synthesis.

09 BIOMASS FUELS↗

NASA NTRS1999

Nondestructive Strain Measurement System Used to Determine Surface Strain on Fibers

Small-diameter structural fibers are being considered as reinforcements for high temperature ceramic matrix composite materials, and thus they require characterization. At the NASA Lewis Research Center, a nondestructive optical technique was used to determine surface strain on a structural fiber, in real time, as it was pulled in a tensile test machine. With this technique, interference or speckle patterns from the laser illuminated fiber test specimen are recorded. As the fiber is pulled, its speckle pattern shifts in proportion to the strain, translation, and rotation components of the sample deformation. Shifting speckle patterns are detected in real time by two linear charge-coupled discharge (CCD) camera arrays, and the images are processed by a hardware correlator. Surface strain is selectively detected on fibers with diameters on the order of 100 mm and can be resolved to 19 microstrain. This system was designed to be robust and compact and generally does not require surface preparation of the structural fibers. For strain detection, two laser beams are positioned incident on the structural fiber being tested, as shown in the photograph, where the test specimen is mounted in a tensile test machine via two coupons. As the fiber is pulled, the speckle pattern produced from each laser beam is detected by one of two CCD arrays located inside the tube on the right side of the photograph.

Tuma, Margaret L.↗

DOE OSTI2024

New dynamic diamond anvil cell for time-resolved radial x-ray diffraction

The dynamic diamond anvil cell (dDAC) is a recently developed experimental platform that has shown promise for studying the behavior of materials at strain rates ranging from intermediate to quasi-static and shock compression regimes. Combining dDAC with time-resolved x-ray diffraction (XRD) in the radial geometry (i.e., with incident x-rays perpendicular to the axis of compression) enables the study of material properties such as strength, texture evolution, and deformation mechanisms. This work describes a radial XRD dDAC setup at beamline P02.2 (Extreme Conditions Beamline) at DESY’s PETRA III synchrotron. Time-resolved radial XRD data are collected for titanium, zirconium, and zircon samples, demonstrating the ability to study the strength and texture of materials at compression rates above 300 GPa/s. In addition, the simultaneous optical imaging of the DAC sample chamber is demonstrated. The ability to conduct simultaneous radial XRD and optical imaging provides the opportunity to characterize plastic strain and deviatoric strain rates in the DAC at intermediate rates, exploring the strength and deformation mechanisms of materials in this regime.

47 OTHER INSTRUMENTATION↗

DOE OSTI2025

Strain-associated nanoscale fluctuating lithium transport within single-crystalline LiNi 1/3 Mn 1/3 Co 1/3 O 2 cathode particles

Solid-state lithium diffusion dynamics are critical for the rate capability and longevity of Li-ion batteries. Conventionally, nanoscale lithium diffusion within individual battery particles has been simplified as being primarily driven by concentration gradients, despite the associated processes inducing local lattice expansion, contraction, and strain fields. Using operando scanning transmission soft X-ray microscopy with high spatial resolution and chemical sensitivity to track nanoscale intraparticle lithium transport, and post-cycling Bragg coherent diffraction X-ray imaging to directly reveal three-dimensional intraparticle strain fields, we uncover strain-associated lithium transport dynamics within single-crystalline LiNi 1/3 Mn 1/3 Co 1/3 O 2 (scNMC) particles during cycling. Contrary to the expected thermodynamic solid-solution behavior of scNMC, our observations reveal near-uniform but fluctuating regions of lithium-dense and lithium-dilute areas during cycling. These fluctuations suggest that nanoscale lithium diffusion can proceed counter to concentration gradients. Additionally, we demonstrate that an increased presence of lithium-dilute regions near the surface enhances lithium surface insertion kinetics, emphasizing the importance of controlling surface lithium distribution to improve rate performance. Our study provides insights into nanoscale solid-state ion transport, with potential applications in batteries, solid-state fuel cells, and memristors.

Lee, Danwon [Seoul National Univ. (Korea, Republic↗

NASA NTRS1999

Investigation of Strain/Vorticity and Large-Scale Flow Structure in Turbulent Nonpremixed Jet Flames

Our study will use the microgravity environment to investigate the underlying flow structure of turbulent nonpremixed round jet flames. In particular, we aim to investigate the large-scale turbulent structure using planar laser Mie scattering (PLMS), and the strain rate and vorticity fields using particle image velocimetry (PIV). This work is motivated by recent studies in our laboratory that have led to several interesting observations of nominally momentum-driven turbulent nonpremixed planar flames. First of all, the organized large-scale turbulent structures that are observed in nonreacting planar jets may be substantially modified or suppressed in nonpremixed planar jet flames. Furthermore, a recent study using PIV and planar laser-induced fluorescence of OH has shown that in transitional and turbulent nonpremixed planar jet flames the presence of the flame seems to greatly influence the underlying vorticity and strain fields, as compared to nonreacting jets. For example, the reaction zones in the jet flames are strongly correlated with regions of high vorticity. A related study has demonstrated that vorticity is not correlated in the same way with either iso-scalar surfaces or scalar dissipation layers in nonreacting planar jets. Furthermore, the relationship between strain and the reaction zone appears to be modified by the presence of high levels of heat release. In particular, the strain rate field in planar jet flames exhibits a preferred direction of principal compressive strain that apparently is related to strong shear across the reaction zone. This preferred direction of strain was not observed in nonreacting jets. One of the major problems encountered when conducting these types of studies is that it is difficult to know to what extent buoyancy influences the results. Therefore, the microgravity environment provides us with an excellent opportunity to explore these issues without the complicating effects of buoyancy. This is particularly the case when studying flames that are transitional between laminar and turbulent states. For example, the strong correlation of vorticity with the reaction zone (discussed above) was observed in both transitional and turbulent planar flames, but the effect was stronger for the transitional case. To date, the reason for the presence of the vorticity-reaction zone correlation is not known, although vorticity production via baroclinic torque is a likely cause. The microgravity environment will allow us to specifically determine whether the vorticity is produced by baroclinic torque resulting from the flame density gradient acting with the hydrostatic pressure gradient.AAdditional details of the planned experiments are provided.

Clemens, N. T.↗

DOE OSTI2021

Strain rate effects on the mechanical behavior of porous titanium with different pore sizes

High strain-rate (up to 6600 s –1 ) and quasi-static compression tests are conducted on a powder-sintered porous titanium with different pore sizes (mean: 30 μm and 120 μm). In situ X-ray imaging is implemented to characterize the pores-scale deformation dynamics. The yield strength as a function of strain rate exhibits two stages of rate sensitivity, and the transition occurs at 1600 s –1 . X-ray images show that pore compaction and strain localizations occur preferentially at pores oriented perpendicular to the loading direction under quasi-static loading, but become more random under high strain-rate loading as a result of higher driving force and plastic deformation nucleation rate. Here, the more homogeneous nucleation of plastic deformation contributes to the increased rate sensitivity beyond 1600 s –1 . At the same strain rate, the yield strength of porous Ti as well as strain field homogeneity decreases significantly with increasing pore size. The small pore spacing in fine-pored Ti reduces the degree of stress concentrations around pores. Therefore, the higher stress concentrations in coarse-pored Ti lead to an earlier yield of matrix around pores and thus a lower bulk yield strength.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Implications of post-processing induced microstructural changes on the deformation and fracture response of additively manufactured Ti–6Al–4V

Ti–6Al–4V parts fabricated via electron beam melting (EBM) powder bed fusion are often subjected to hot isostatic pressing below the β-transus temperature to mitigate defects. During which the pressure aids in pore closure and the thermal exposure results in coarsening of α phase while retaining the columnar prior-β phase grain morphology present in the as-fabricated condition. The same post-processing treatment can also be carried out above β-transus temperature which is an effective way to modify both the grain morphology and the associated α textures. Here, the objective of this work is to correlate thermally induced microstructural changes to the deformation and fracture response of the EBM processed Ti–6Al–4V. To this end, we have carried out both sub-transus and super-transus heat-treatments of the as-fabricated material. The mechanical response of the as-fabricated and all heat-treated materials are characterized by in-situ tensile tests under a high-resolution digital optical microscope. This enabled us to capture large-scale panoramic images of the deforming microstructure, and overcome the trade-off between the image resolution and the field of view during in-situ experiments. The series of images captured throughout the imposed deformation are subsequently used to perform microstructure-based digital image correlation to measure microstructural-scale strains over a large area. The results of the in-situ tests together with detailed fractographic analyses are then used to elucidate how the heterogeneous deformation spanning over multiple microstructural length-scales, for example, at the scale of lamellae, colonies of lamellae and grain boundaries, affect the overall deformation and fracture response of the post-processed materials.

36 MATERIALS SCIENCE↗

DOE OSTI2024

New dynamic diamond anvil cell for time-resolved radial x-ray diffraction

47 OTHER INSTRUMENTATION↗

DOE OSTI2021

Burst characteristics of advanced accident-tolerant FeCrAl cladding under temperature transient testing

Here assessment of burst characteristics of accident-tolerant fuel (ATF) claddings is essential to evaluate the safety margins of nuclear reactors, and better understanding can enable accelerated licensing for reactor concepts that include the new materials. Therefore, this study investigated the burst behavior of an ATF candidate of C26M, which is an iron–chromium–aluminum alloy (FeCrAl) under transient testing like the simulated loss-of-coolant accident (LOCA) conditions, except the water-quenching phase, in light-water reactors (LWRs). The effect of LOCA specimen length was assessed in terms of post-burst tube parameters. No critical length effect was determined on the burst pressure, burst location, and burst size measurements. Burst temperature showed larger variation likely due to its measurement approach used in this study. The post-test diametral strain was identified as the critical parameter to reduce the specimen length as compared to tube burst length or width. Postmortem optical metrology and digital image correlation were employed to determine the local strain-state during the simulated LOCA, which showed the loading path was close to equibiaxial conditions in regions away from the burst location, rather than internally pressurized conditions (or “plane-strain” tension). Pst-test microstructural characterizations of the FeCrAl revealed that ductile damage was present at the edge of the outer radial surface while the rest of the material was ruptured via cleavage at LOCA burst temperatures. Furthermore, internal grain boundary cracks were observed at locations away from the tube burst region. This behavior was considered to occur during the cooling down period of the simulated LOCA test. Overall, this study aimed to provide essential data for fuel performance code development by considering micromechanics of the deformation and failure.

36 MATERIALS SCIENCE↗