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At least 1,171 records · Page 65

Synthesis and characterization of electron beam irradiation-induced damage in polycrystalline metal thin films

High-energy physics research, industrial sterilizing, and material processing depend extensively on electron beam accelerators. Exit windows are crucial components of such electron accelerator systems, maintaining vacuum integrity inside the machine while providing mechanical strength, thermal stability, and radiation resistance at the beam-target interface. In this study, thin metallic films of Ni, Ti, Cr, and V were explored for use in electron beam exit windows, and their properties were compared with the properties of their bulk counterparts. Simulation results of metal foils predicted Ti to exhibit less beam power dissipation compared to Ni. However, Ni possesses superior mechanical and structural properties compared to Ti. The performance of these films under electron beam irradiation was examined by depositing thin layers of these films on silicon and metallic substrates using magnetron sputtering and exposing them to e-beam irradiation in a controlled setup. The deposited films were subjected to a dose of approximately 66 kGy at a beam energy of 10 MeV and characterized prior to and postexposure to the beam using field emission scanning electron microscopy, atomic force microscopy, x-ray diffraction (XRD), and nanoindentation. Particular emphasis was given to characteristics like the grain structure, surface morphology, dislocation density, and hardness. XRD patterns revealed irradiation-induced changes in peak intensities, while the crystallinity remained largely unchanged. Nanoindentation results showed that the pristine and irradiated Ti and Ni films were twice as hard when compared to bulk Ti and Ni samples, regardless of the substrate type used (Si or bulk Ti, or Ni). These results emphasize the superior mechanical properties of thin metal films compared to their bulk counterparts. In conclusion, this study advances the optimization of thin film materials for robust and efficient e-beam applications, ensuring improved durability and operational reliability.

AFM↗

Ultrasonic waveguide reflectometry for quench detection (CRADA Final Report)

Early detection of thermal runaway (quench) is critical for safely operating high-temperature superconductor (HTS) magnets. Voltage-based techniques provide late detection of quenching in HTS, which can lead to magnet burnout and system damage. Various non-voltage quench-detection approaches are therefore investigated nowadays that are based on magnetic, acoustic, and optical sensing. LBNL has been actively developing the quench detection principle based on diffuse ultrasonic wave propagation since 2017 and has demonstrated the approach's viability with several peer-reviewed publications and a patent application. Over the last decade, Etegent, LBNL partner for this proposal and effort, has been developing a sensing technology that utilizes the propagation of stress waves through the solid metallic and nonmetallic waveguides (WG). The method is based on the dependence of materials' elastic properties and the speed of sound on temperature. Compared with optical analog, acoustic WG operates at much lower frequencies, eliminating the need for expensive, complex, highly sensitive receivers and data processing. Etegent proved this technology in many harsh environments, mainly concentrated high-temperature measurements. The initial contact between LBNL and Etegent started in 2020, aiming at combining our knowledge and effort toward developing a viable ultrasound-based quench detection technique for use with HTS magnets. A preliminary study conducted jointly in 2022 found no principle restrictions for expanding the WG technology toward cryogenic temperature operation. The present CRADA work aimed at designing, building, and testing ultrasonic waveguide temperature sensors at relevant cryogenic conditions, and demonstrating this technology's applicability to detecting heating and quenching in High Temperature Superconductor (HTS)-based cables and magnets. The technical objectives of the project included: (1) Design and fabricate ultrasonic WG sensors suitable for cryogenic operation, (2) Test ultrasonic WGs under cryogenic conditions, (3) Determining a suitable way of insulating WGs to prevent ultrasonic leakage while maintaining good thermal contact with the surrounding medium, (4) WG integration and cryogenic test with HTS conductors and HTS magnets, and (5) Design and basic prototyping of a standalone WG-based quench detection system. This project adds value to the present LBNL magnet diagnostics portfolio and enables a breakthrough in addressing the HTS magnet quench detection challenge.

47 OTHER INSTRUMENTATION↗

Multiple Degradation Mechanisms in Reinforced Concrete Structures, Modeling and Risk Analysis

The overarching goal of this project is to complement ongoing Department of Energy (DOE) Light Water Reactor Sustainability (LWRS)-funded Grizzly concrete modeling development efforts by providing improved multi-physics models for incorporation into the Grizzly and BlackBear codes. Objectives of this work identified at the outset of this project include: 1. Coupling between mechanical damage and transport processes. The mechanical damage will be characterized by nonlinear mechanical constitutive models appropriate for concrete used in nuclear power plants (NPPs). 2. Improved representation of the coupling among the transport process, building on the current moisture and thermal transport models in Grizzly. The parameters for coupling among heat and mass transport in the multi-physics model will be experimentally determined. 3. Coupling among different scale levels of concrete constituents, fine and coarse aggregates, cement paste, hydration products, and pore structure. 4. Probabilistic analysis of the random nature of the heterogeneous concrete structure and the environmental factors (ambient temperature and humidity) and their multiple effects on concrete deterioration. 5. Benchmark verification, validation and uncertainty quantification of the thermo-hygro- chemo-mechanical (THCM) concrete formulation. The end goal of this work was to provide a comprehensive and robust simulation capability that can be applied at the engineering scale for analysis of realistic deterioration scenarios in NPP concrete structures.

36 MATERIALS SCIENCE↗

Multiphysics Simulations of Nanofibrous High Power Targets for the Inference of Failure Modes

Fermilab s High Power Targetry Research and Development (HPT R&D) group have been developing and studying an electrospun nanofiber target concept to support the need for robust targets in future fixed target facilities. These nanofiber mats have demonstrated resistance to radiation damage, and the free motion of the individual fibers is expected to mitigate the cyclic stresses induced by a pulsed, high-power beam. To evaluate the efficacy of this concept, nanofiber mat samples have been sent by the HPT R&D group to the HiRadMat facility at CERN for prototypic thermal shock testing; the outcomes of these experiments show that the survivability of a nanofiber target depends on its construction parameters, in particular the packing density of the fibers. Samples with higher packing densities have consistently been destroyed by exposure to the HiRadMat beam, with a hole at the beam center visible, and layers of nanofibers peeled away from the center hole, whereas samples with lower densities have survived with limited damage. The exact reason for the failure of the higher density targets was unclear at the time of the original experiments, but the results of our recent multiphysics simulations which recreate the experiments support the hypothesis that the expansion and pressurization of the air inside the target after being heated by the pulsed beam is the cause; in a high density nanofiber mat, the motion of air through the pores of the mat is much more restricted, and induces a larger pressure on the fibers, blowing the mat apart. In this talk, we ll share the results of these simulations and discuss how they support this hypothesis.

Asztalos, Will↗

Microcracking in composite laminates under thermal and mechanical loading

Composites used in space structures are exposed to both extremes in temperature and applied mechanical loads. Cracks in the matrix form, changing the laminate thermoelastic properties. The goal of the present investigation is to develop a predictive methodology to quantify microcracking in general composite laminates under both thermal and mechanical loading. This objective is successfully met through a combination of analytical modeling and experimental investigation. In the analysis, the stress and displacement distributions in the vicinity of a crack are determined using a shear lag model. These are incorporated into an energy based cracking criterion to determine the favorability of crack formation. A progressive damage algorithm allows the inclusion of material softening effects and temperature-dependent material properties. The analysis is implemented by a computer code which gives predicted crack density and degraded laminate properties as functions of any thermomechanical load history. Extensive experimentation provides verification of the analysis. AS4/3501-6 graphite/epoxy laminates are manufactured with three different layups to investigate ply thickness and orientation effects. Thermal specimens are cooled to progressively lower temperatures down to -184 C. After conditioning the specimens to each temperature, cracks are counted on their edges using optical microscopy and in their interiors by sanding to incremental depths. Tensile coupons are loaded monotonically to progressively higher loads until failure. Cracks are counted on the coupon edges after each loading. A data fit to all available results provides input parameters for the analysis and shows them to be material properties, independent of geometry and loading. Correlation between experiment and analysis is generally very good under both thermal and mechanical loading, showing the methodology to be a powerful, unified tool. Delayed crack initiation observed in a few cases is attributed to a lack of preexisting flaws assumed by the analysis. Some interactions between adjacent ply groups are attributed to local stress concentrations. These two effects are not captured by the analysis due to its global nature. The analysis is conservative in these cases and agrees well with data after the observed onset of cracking.

Maddocks, Jason R.↗

Worldwide Physics-Based Lifetime Prediction of c-Si Modules Due to Solder-Bond Failure

Lifetime prediction of the fielded c-Si solar modules due to location-specific weather conditions has been an important topic of photovoltaic research and the economic viability of solar energy. Data analytic techniques such as the performance ratio method, Statistical clear sky model, and Suns-Vmp methods quantify the degradation from measured data of a solar farm, however, the nonlinear time-dependence and correlated degradations make it difficult to use the empirical degradation rates for ultimate lifetime projection. In this article, we propose a complementary physics-based model to predict the solder bond failure caused by mechanical stress associated with the variations of the temperature. Integrating the worldwide weather information from NASA/NSRDB databases, the model predicts the location-specific output-power degradation and the lifetime of a module due to solder bond failure. The model parameters are calibrated against qualification tests involving thermal cycling of specific batches of modules from a specific technology/manufacturer. The results may be summarized as: 1) Modules installed at higher latitudes show a longer lifetime due to reduced damage accumulation. 2) The reduction of temperature fluctuation close to large bodies of water, such as seashores, increases solder bond lifetime significantly. 3) Relatively speaking, modules installed close to the Tropic of Cancer/Capricorn (23.5 degrees North/South) suffer from a higher solder bond damage and have a shorter lifetime, suggesting a conservative design. This model should serve as a building block of a comprehensive reliability framework that can predict the lifetime of a module that experiences simultaneous and correlated degradation mechanisms involving yellowing, corrosion, and potential-induced degradation.

14 SOLAR ENERGY↗

Salt Tank Testbed: a Test Site Designed to Replicate Floor Buckles Observed in Commercial TES Tanks

A test site has been designed and is under construction to replicate the buckling failure ob-served in several in-service storage tanks for nitrate salts operating up to 565°C. In commercial tanks multiple factors have been identified that influence the floors susceptibility to buck-ling, including: the as-manufactured shape of the floor, high compressive stresses due to thermal gradients and/or friction, fluid inventory and absolute temperature. Based on exten-sive modeling analysis it was determined that similar buckles can be reproduced in a scaled test tank (approximately 9x smaller than a representative commercial tank design). To buckle the scaled tank a radial thermal gradient is generated in the tank with a low fluid level, the fluid level is then increased while maintaining the thermal gradient; based on the modeling results just one of these cycles can plastically deform the tank floor. The test site which is under construction is designed to replicate this damaging cycle at lower temperatures. The goal of testing will be to reproduce this damaging cycle and buckle the scaled test tank floor, allowing proper model validation and a methodology for comparing different tank designs at a smaller (and less costly) scale.

25 ENERGY STORAGE↗

Initial Feasibility Assessment and Broader Strategy Development for Fiber Integration via Advanced Manufacturing

Structural health monitoring is critical for ensuring the operational safety and cost-competitiveness of the developing advanced reactor designs. The extreme operational envelopes of these advanced architectures, having operating temperatures ranging 400°C–1,000°C and heightened displacement damage doses, render conventional commercially available piezoelectric transducers and resistive strain gauges unviable. Optical fiber sensors present an attractive solution for advanced radiation-hardened instrumentation due to their high thermal stability and distributed sensing capabilities. However, their deployment in embedded applications can be hindered by the severe thermomechanical strain driven by the coefficient of thermal expansion mismatch between fused silica glass and structural metal alloys like stainless steel (e.g., SS316L).

36 MATERIALS SCIENCE↗

Methods of measurement for semiconductor materials, process control, and devices

Activities directed toward the development of methods of measurement for semiconductor materials, process control, and devices are described. Topics investigated include: measurements of transistor delay time; application of the infrared response technique to the study of radiation-damaged, lithium-drifted silicon detectors; and identification of a condition that minimizes wire flexure and reduces the failure rate of wire bonds in transistors and integrated circuits under slow thermal cycling conditions. Supplementary data concerning staff, standards committee activities, technical services, and publications are included as appendixes.

Bullis, W. M.↗

Thermally induced stresses and deformations in layered composite tubes

The thermally induced stresses and deformations in layered, orthotropic tubes are studied. The motivation for studying tubes is their likely application for use in space structures. Tubes are a strong candidate for this application because of their high structural efficiency, as measured by stiffness per unit weight, and their relative ease of fabrication. Also, tubes have no free edges to deteriorate or delaminate. An anticipated thermal condition for tubes in space is a circumferential temperature gradient. This type of gradient will introduce dimensional changes into the structure and may cause stresses large enough to cause damage to the material. There are potentially large differences in temperatures at different circumferential locations on the tube. Because of this, the effects of temperature dependent material properties on the stresses and deformations may be important. The study is composed of three parts: experiments to determine the functional form of the circumferential gradient and to measure tube deflections; an elasticity solution to compute the stresses and deformations; and an approximate approach to determine the effects of temperature dependent material properties.

Cooper, D. E.↗

Fiber composite structural durability and damage tolerance: Simplified predictive methods

Simplified predictive methods and models (theory) to evaluate fiber/polymer-matrix composite material for determining structural durability and damage tolerance are presented and described. This theory includes equations for (1) fatigue and fracture of composites without and with defects, (2) impact resistance and residual strength after impact, (3) thermal fatigue, and (4) combined stress fatigue. Several examples are included to illustrate applications of the theory and to identify significant parameters and sensitivities. Comparisons with limited experimental data are made.

Chamis, Christos C.↗

Fiber composite structural durability and damage tolerance - Simplified predictive methods

Simplified predictive methods and models (theory) to evaluate fiber/polymer-matrix composite material for determining structural durability and damage tolerance are presented and described. This theory includes equations for (1) fatigue and fracture of composites without and with defects, (2) impact resistance and residual strength after impact, (3) thermal fatigue, and (4) combined stress fatigue. Several examples are included to illustrate applications of the theory and to identify significant parameters and sensitivities. Comparisons with limited experimental data are made.

Chamis, Christos C.↗

Mechanical Characterization of Thermomechanical Matrix Residual Stresses Incurred During MMC Processing

In recent years, much effort has been spent examining the residual stress-strain states of advanced composites. Such examinations are motivated by a number of significant concerns that affect composite development, processing, and analysis. The room-temperature residual stress states incurred in many advanced composite systems are often quite large and can introduce damage even prior to the first external mechanical loading of the material. These stresses, which are induced during the cooldown following high-temperature consolidation, result from the coefficient of thermal expansion mismatch between the fiber and matrix. Experimental techniques commonly used to evaluate composite internal residual stress states are non-mechanical in nature and generally include forms of x-ray and neutron diffraction. Such approaches are usually complex, involving a number of assumptions and limitations associated with a wide range of issues, including the depth of penetration, the volume of material being assessed, and erroneous effects associated with oriented grains. Furthermore, and more important to the present research, these techniques can assess only "single time" stress in the composite. That is, little, if any, information is obtained that addresses the time-dependent point at which internal stresses begin to accumulate, the manner in which the accumulation occurs, and the presiding relationships between thermoelastic, thermoplastic, and thermoviscous behaviors. To address these critical issues, researchers at the NASA Lewis Research Center developed and implemented an innovative mechanical test technique to examine in real time, the time-dependent thermomechanical stress behavior of a matrix alloy as it went through a consolidation cycle.

Castelli, Michael G.↗

Hail Disrometer Array for Launch Systems Support

Prior to launch, the space shuttle might be described as a very large thermos bottle containing substantial quantities of cryogenic fuels. Because thermal insulation is a critical design requirement, the external wall of the launch vehicle fuel tank is covered with an insulating foam layer. This foam is fragile and can be damaged by very minor impacts, such as that from small- to medium-size hail, which may go unnoticed. In May 1999, hail damage to the top of the External Tank (ET) of STS-96 required a rollback from the launch pad to the Vehicle Assembly Building (VAB) for repair of the insulating foam. Because of the potential for hail damage to the ET while exposed to the weather, a vigilant hail sentry system using impact transducers was developed as a hail damage warning system and to record and quantify hail events. The Kennedy Space Center (KSC) Hail Monitor System, a joint effort of the NASA and University Affiliated Spaceport Technology Development Contract (USTDC) Physics Labs, was first deployed for operational testing in the fall of 2006. Volunteers from the Community Collaborative Rain. Hail, and Snow Network (CoCoRaHS) in conjunction with Colorado State University were and continue to be active in testing duplicate hail monitor systems at sites in the hail prone high plains of Colorado. The KSC Hail Monitor System (HMS), consisting of three stations positioned approximately 500 ft from the launch pad and forming an approximate equilateral triangle (see Figure 1), was deployed to Pad 39B for support of STS-115. Two months later, the HMS was deployed to Pad 39A for support of STS-116. During support of STS-117 in late February 2007, an unusual hail event occurred in the immediate vicinity of the exposed space shuttle and launch pad. Hail data of this event was collected by the HMS and analyzed. Support of STS-118 revealed another important application of the hail monitor system. Ground Instrumentation personnel check the hail monitors daily when a vehicle is on the launch pad, with special attention after any storm suspected of containing hail. If no hail is recorded by the HMS, the vehicle and pad inspection team has no need to conduct a thorough inspection of the vehicle immediately following a storm. On the afternoon of July 13, 2007, hail on the ground was reported by observers at the VAB, about three miles west of Pad 39A, as well as at several other locations around Kennedy Space Center. The HMS showed no impact detections, indicating that the shuttle had not been damaged by any of the numerous hail events which occurred that day.

Lane, John E.↗

In situ cryogenic characterization of proton damage in thick p-channel skipper CCDs

Skipper charge-coupled devices (CCDs) are an offshoot of standard silicon pixel detectors and are capable of performing repeated non-destructive charge measurements, enabling deeply sub-electron readout noise. This capability has opened the door to single-photon counting from the near-infrared ($\sim$1.1 $μ$m) to the soft X-ray (several keV), making these devices strong candidates for future astronomical instruments operating in the photon-starved limit. Furthermore, the p-channel architecture used to fabricate Skipper CCDs on n-type silicon has been demonstrated to have an increased hardness to the intense radiation environment of space. Building upon previous irradiation campaigns on room-temperature sensors, here we describe the first radiation-hardness tests of p-channel skipper CCDs at their cryogenic operating temperatures. We assess the performance of the floating-gate output stage and global CCD parameters (charge transfer inefficiency, dark current, hot pixels, and charge traps). We find that these devices maintain excellent performance after displacement damage doses equivalent to ${\sim}$10 years at the Earth/Sun L2 Lagrange point, demonstrating for the first time that these sensors remain radiation-hard in realistic deep-space thermal and radiation environments.

Roach, Brandon M. [Chicago U., KICP] (ORCID:000000↗

Space environmental effects on LDEF composites: A leading edge coated graphite epoxy panel

The electronics module cover for the leading edge (Row D 9) experiment M0003-8 was fabricated from T300 graphite/934 epoxy unidirectional prepreg tape in a (O(sub 2), +/- 45, O(sub 2), +/- 45, 90, 0)(sub s) layup. This 11.75 in x 16.75 in panel was covered with thermal control coatings in three of the four quadrants with the fourth quadrant uncoated. The composite panel experienced different thermal cycling extremes in each quadrant due to the different optical properties of the coatings and bare composite. The panel also experienced ultraviolet (UV) and atomic oxygen (AO) attack as well as micrometeoroid and space debris impacts. An AO reactivity of 0.99 x 10(exp -24) cm(sup 3)/atom was calculated for the bare composite based on thickness loss. The white urethane thermal control coatings (A276 and BMS 1060) prevented AO attack of the composite substrate. However, the black urethane thermal control coating (Z306) was severely eroded by AO, allowing some AO attack of the composite substrate. An interesting banding pattern on the AO eroded bare composite surface was investigated and found to match the dimensions of the graphite fiber tow widths as prepregged. Also, erosion depths were greater in the darker bands. Five micrometeoroid/space debris impacts were cross sectioned to investigate possible structural damage as well as impact/AO interactions. Local crushing and delaminations were found to some extent in all of the impacts. No signs of coating undercutting were observed despite the extensive AO erosion patterns seen in the exposed composite material at the impact sites. An extensive microcrack study was performed on the panel along with modeling of the thermal environment to estimate temperature extremes and thermal shock. The white coated composite substrate displayed almost no microcracking while the black coated and bare composite showed extensive microcracking. Significant AO erosion was seen in many of the cracks in the bare composite.

George, Pete E.↗

ELASTOMERIC MICROVASCULAR SELF-HEALING MATERIALS

Damaged elastomeric diaphragms within pneumatic controllers used in the oil and gas industry lead to an unintended release of methane. Self-healing microvascular materials capable of healing various types of damage have been fabricated. These microvascular materials are designed to replace currently available commercial diaphragms found in pneumatic controllers and provide a solution to reduce unintended methane leaks. Poly(dimethylsiloxane) (PDMS) was used as the main matrix material, with additional testing conducted on polyurethane and flexibilised epoxy materials. Microvascular networks were implemented into the elastomeric membranes to act as ves- sels to deliver healing agents to the damaged areas. The complex, interdigitated channel networks were created using a 3D printed custom compounded filament composed of polylactic acid (PLA) and tin(II) oxalate. Two-part liquid casting polymers were poured around the channels into a mould to create samples with the scaffolding of the microvascular channels intact. Hollow microvascular networks were created by placing the samples within a vacuum oven at 250◦C which causes the thermal depolymerisation of PLA into its gaseous monomers. The manufactured materials were placed in test stands and pressurized using nitrogen gas to determine their healing and mechanical behaviour. Self-healing behaviour was demonstrated using PDMS matrix materials and healing chemistries within a pressure test cell. This test cell was designed to detect any damage to a sample by record- ing an outlet pressure. Damages including puncture holes, diagonal cuts and star-shaped central iv cuts were applied to the samples and a reduction in the outlet pressure was recorded for all sam- ples. A variation in channel spacing and diameter was studied to determine the optimal design of the microvascular network for self-healing performance. The mechanical performance of elastomeric membrane materials within a diaphragmatic pressurised stand was observed. Deformations and strains around the channels and channel inter- sections at the midplane of the materials were recorded using digital image correlation. Normal stresses were calculated using Hooke’s law and the material properties of the PDMS matrix. A reduction in leak rate, implying the success of self-healing, was recorded within manu- factured diaphragm samples tested within a commercial valve. PDMS is the favourable material when compared to polyurethane and flexibilised epoxy for creating

03 NATURAL GAS↗

Thermoresponsive polymer assemblies via variable temperature liquid-phase transmission electron microscopy and small angle X-ray scattering

Abstract Herein, phase transitions of a class of thermally-responsive polymers, namely a homopolymer, diblock, and triblock copolymer, were studied to gain mechanistic insight into nanoscale assembly dynamics via variable temperature liquid-cell transmission electron microscopy (VT-LCTEM) correlated with variable temperature small angle X-ray scattering (VT-SAXS). We study thermoresponsive poly(diethylene glycol methyl ether methacrylate) (PDEGMA)-based block copolymers and mitigate sample damage by screening electron flux and solvent conditions during LCTEM and by evaluating polymer survival via post-mortem matrix-assisted laser desorption/ionization imaging mass spectrometry (MALDI-IMS). Our multimodal approach, utilizing VT-LCTEM with MS validation and VT-SAXS, is generalizable across polymeric systems and can be used to directly image solvated nanoscale structures and thermally-induced transitions. Our strategy of correlating VT-SAXS with VT-LCTEM provided direct insight into transient nanoscale intermediates formed during the thermally-triggered morphological transformation of a PDEGMA-based triblock. Notably, we observed the temperature-triggered formation and slow relaxation of core-shell particles with complex microphase separation in the core by both VT-SAXS and VT-LCTEM.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗