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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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Effect of Prolonged Ultraviolet Radiation Exposure on the Blast Response of Fiber Reinforced Composite Plates

An experimental study with corresponding numerical simulations was conducted to evaluate the blast response of composite plates after prolonged exposure to ultraviolet radiation. Two composite materials were used in this study, namely carbon fiber/epoxy and glass fiber/vinyl ester. The composite materials consisted of four unidirectional fiber plies oriented in a [± 45°]s layup. The plates were placed in a QUV Accelerated Weathering Tester for 500 h of exposure on each face, totaling 1000 h of ultraviolet radiation exposure, equivalent to 2.5 MJ/m{sup 2} of energy. The QUV Accelerated Weathering Tester was equipped with eight UVA-340 lamps to provide real service life exposure conditions. Material characterization experiments were performed on virgin specimens, as well as specimens exposed to ultraviolet radiation for 1000 h to determine its effect on the mechanical properties of the composites. Blast experiments were conducted on the composite plates to investigate the dynamic response before and after exposure to ultraviolet radiation. The plates were clamped on all edges and subjected to an air blast using a shock tube apparatus. Three-dimensional digital image correlation was coupled with high-speed photography to obtain full-field displacements of the specimens during blast loading. Furthermore, three piezoelectric pressure transducers were mounted on the shock tube apparatus and utilized to measure the pressure history of the shock wave loading. The quasi-static material characterization showed that the tensile modulus E{sub 1} had minimal change after exposure to ultraviolet radiation for 1000 h. However, matrix-dominated properties such as the in-plane shear modulus G{sub 12} increased after exposure to ultraviolet light for both the carbon and glass fiber composites, which resulted in lower out-of-plane displacements during blast loading. For the carbon fiber plates, the forced vibration frequency induced by the transverse blast load was higher in plates exposed to ultraviolet radiation when compared to virgin specimens. However, for the glass fiber plates exposed to ultraviolet radiation, the forced vibration frequency decreased when compared to virgin specimens. Finally, the finite element simulations were in good agreement with the experimental results. The simulations revealed that the glass fiber plates exposed to ultraviolet radiation had higher failure strains at the boundary than virgin specimens, despite having higher stiffness. A parametric study in which higher loading was simulated also showed that the glass fiber plates experienced more damage after 1000 h of ultraviolet radiation exposure.

36 MATERIALS SCIENCE↗

A shock tube with a high-repetition-rate time-of-flight mass spectrometer for investigations of complex reaction systems

A conventional membrane-type stainless steel shock tube has been coupled to a high-repetition-rate time-of-flight mass spectrometer (HRR-TOF-MS) to be used to study complex reaction systems such as the formation of pollutants in combustion processes or formation of nanoparticles from metal containing organic compounds. Opposed to other TOF-MS shock tubes, our instrument is equipped with a modular sampling unit that allows to sample with or without a skimmer. The skimmer unit can be mounted or removed in less than 10 min. Thus, it is possible to adjust the sampling procedure, namely, the mass flux into the ionization chamber of the HRR-TOF-MS, to the experimental situation imposed by species-specific ionization cross sections and vapor pressures. The whole sampling section was optimized with respect to a minimal distance between the nozzle tip inside the shock tube and the ion source inside the TOF-MS. The design of the apparatus is presented and the influence of the skimmer on the measured spectra is demonstrated by comparing data from both operation modes for conditions typical for chemical kinetics experiments. The well-studied thermal decomposition of acetylene has been used as a test system to validate the new setup against kinetics mechanisms reported in literature.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Diaphragmless single-pulse shock tube for high-temperature chemical kinetics studies

Single-pulse shock tubes are effective tools for measuring chemical kinetics at high temperatures, typically (900–1400) K. However, the use of a diaphragm for shock generation leads to significant shock-to-shock inconsistencies in temperature for a constant initial pressure ratio across the discontinuity. Diaphragms also require replacement after each shock and demand care in cleaning to ensure that the fragments do not contaminate the apparatus. A piston-driven valve design is presented that leads to a highly reproducible postreflected shock temperatures (0.41% at 1147 K and 0.61% at 967 K) in a single pulse varying from (500 to 1200) µs in width over the temperature range of interest. Characterization of the valve was accomplished using both shock-speed measurements and independent measurements of the pulse temperature using reference thermal decomposition reactions.

47 OTHER INSTRUMENTATION↗

Note: An improved driver section for a diaphragmless shock tube

Improvements to equipment lifetime and measurement reproducibility have been made by modifying the actuating mechanism of a diaphragmless shock tube that is used for high temperature gas kinetic studies. We report the modifications have two major benefits while retaining the simplicity of the original apparatus. First, the reproducibility of shock wave generation has been greatly improved and is demonstrated with 50 nearly identical experiments on the dissociation of cyclohexene at T 2 = 1765 ± 13 K and P 2 = 120 ± 1 Torr, demonstrating the capability for signal averaging over many experiments. Second, the lifetime of the bellows which forms the heart of the actuator is considerably improved, significantly increasing the time between replacements.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

High-speed laser-launched flyer impacts studied with ultrafast photography and velocimetry

Pulsed lasers can launch thin metal foils at km s -1 , but for precision measurements in shock compression science and shock wave spectroscopy, where one-dimensional shock compression is vital, flyer plate impacts with targets must have a high degree of flatness and minimal tilt, and the flyer speeds and impact times at the target must be highly reproducible. We have developed an apparatus that combines ultrafast stroboscopic optical microscopy with photon Doppler velocimetry to study impacts of laser-launched Al and Cu flyer plates with flat, transparent glass targets. The flyer plates were 0.5 mm in diameter, and ranged from 12-100 μm thick, with flyer speeds up to 6.25 km s -1 . The velocity variations over 30-60 launches from the same flyer plate optic can be as low as 0.6%, and the impact time variations can be as low as 0.8 ns. Stroboscopic image streams (reconstructed movies) show uniform, flat impacts with a glass target. As a result, these stroboscopic images can be used to estimate the tilt in the flyer-target impact to be <1mrad.

36 MATERIALS SCIENCE↗

Ejected particle size measurement using Mie scattering in high explosive driven shockwave experiments

In this paper, we report on the development of a diagnostic to provide constraints on the size of particles ejected from shocked metallic surfaces. The diagnostic is based on measurements of the intensity of laser light transmitted through a cloud of ejected particles as well as the angular distribution of scattered light, and the analysis of the resulting data is done using the Mie solution. Finally, we describe static experiments to test our experimental apparatus and present initial results of dynamic experiments on Sn targets. Improvements for future experiments are briefly discussed.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Laboratory system for studying cryogenic thermal rock fracturing for well stimulation

The concept of cryogenic fracturing is that a sharp thermal gradient developed by applying a cryogenic fluid on a rock surface causes a strong local tensile stress that initiates fractures. Prior field tests suggest that field application with special equipment rated for cryogenic temperatures may deliver potential benefits. The tests did not, however, identify the fracture mechanisms at work in downhole conditions. We present our laboratory designs and procedures developed for studying cryogenic fracturing mechanisms in a well environment, and examine typical data indicative of the performance of the system. The experimental apparatus and procedures were specifically designed to conduct cryogenic fracturing tests in specimens under confining stress, with integrated cryogen transport, measurements, and fracture characterization. A true-triaxial loading system was built to simulate reservoir stress levels and anisotropic stress application, and was designed to avoid thermal stresses in tests involving cryogen by arranging discrete components in an open chamber. To maximize thermal shock on the wellbore surface, tubing and wellhead are configured so that liquid nitrogen enters the borehole and flow out after contributing to thermal shock. The temperature at boreholes and along flow lines, borehole pressure, and liquid nitrogen consumption are monitored throughout treatments. Acoustic transmission and pressure-decay measurements are used to characterize fractures before and after the experiments. Breakdown tests performed on un-stimulated specimens and stimulated specimens compare breakdown pressures of the two groups and thus evaluate the performance of thermal fracturing. The laboratory design was able to effectively apply cryogenic stimulations to laboratory rock specimens. Finally, the characterization methods were able to capture fracture creation and rock property changes due to cryogenic fracturing.

54 ENVIRONMENTAL SCIENCES↗

Failure of brittle micro-spherical shells embedded in elastomer matrix under indentation

Silicone elastomer filled with glass micro balloons (GMB) is an elastomeric syntactic foam used in electronics and component packaging for encapsulation, potting, stress-relief layer, and electrical insulation purposes. Under mechanical loading, the reinforcing phase, namely the GMBs embedded in the elastomer matrix, may break or delaminate, leading to internal damage and macroscale stiffness degradation, which can alter the material's protective capacity against mechanical shock and vibration. The degree of damage is controlled by the loading history, delamination, and failure behavior of the GMBs. In this work, we investigate the GMB failure behavior in this work wherein we present an indentation experiment to measure the force required to fail individual GMBs that are either embedded in the elastomer matrix or adhered to the surface of an elastomer layer. The indentation apparatus is augmented with an inverted optical microscope to enable in situ imaging of the GMB. Failure modes for the embedded or non-embedded GMBs are discussed based on the morphology of the broken GMBs and the measured failure forces. We also measure the adhesion energy between the glass balloon and the elastomer, based on which the possibility of delamination between the GMB and the surrounding elastomer matrix during the failure process is evaluated. Our results can facilitate the development of a failure criterion of GMBs which is necessary for establishing a physics-based constitutive model to describe the macroscopic damage mechanics of elastomeric syntactic foams.

42 ENGINEERING↗

Femtosecond Reflectance Spectroscopy for Energetic Material Diagnostics

Understanding the fundamental mechanisms underpinning shock initiation is critical to predicting energetic material (EM) safety and performance. Currently, the timescales and pathways by which shock-excited lattice modes transfer energy into specific chemical bonds remains an open question. Towards understanding these mechanisms, our group has previously measured the vibrational energy transfer (VET) pathways in several energetic thin films using broadband, femtosecond transient absorption spectroscopy. However, new technologies are needed to move beyond these thin film surrogates and measure broadband VET pathways in realistic EM morphologies. Herein, we describe a new broadband, femtosecond, attenuated total reflectance spectroscopy apparatus. Performance of the system is benchmarked against published data and the first VET results from a pressed EM pellet are presented. This technology enables fundamental studies of VET dynamics across sample configurations and environments (pressure, temperature, etc .) and supports the potential use of VET studies in the non-destructive surveillance of EM components.

42 ENGINEERING↗

Insight into the Chemistry of PETN Under Shock Compression Through Ultrafast Broadband Mid-Infrared Absorption Spectroscopy

In this study, thin films of pentaerythritol tetranitrate (PETN) were shock compressed using the laser driven shock apparatus at Los Alamos National Laboratory (LANL). Two spectroscopic probes were available to this apparatus: visible white light transient absorption spectroscopy (VIS) from 400 to 700 nm and mid-infrared transient absorption spectroscopy (MIR) from 1150 to 3800 cm –1 . Important PETN vibrational modes are the symmetric and antisymmetric NO 2 stretches at 1280 and 1650 cm –1 , respectively, as well as CH stretches at ~2900 cm –1 . Shock strength was varied from approximately 3 to 55 GPa to span from the chemically unreactive regime to the regime in which fast chemical reaction took place on the 250 ps time scale of the measurements. VIS and MIR results suggest irreversible chemistry was induced in PETN at pressures above 30 GPa. At lower shock pressures, the spectroscopy showed minimal changes attributable to pressure induced effects. Under the higher-pressure reactive conditions, the frequency region at the antisymmetric NO 2 stretch mode had a significantly increased absorption while the region around the symmetric NO 2 stretch did not. No observable increased absorption occurred in the higher frequency regions where CH-, NH-, and OH- bond absorptions would be observed. A broad absorption appeared on the shoulder at the red-edge of the CO 2 vibrational band around 2200 cm –1 . In addition to the experiments, reactive molecular dynamics were carried out under equivalent shock conditions to correlate the evolution of the infrared spectrum to molecular processes. The simulations show results consistent to experiments up to 30 GPa but suggest that NO and NO 2 related features provided the strongest contributions to the shocked infrared changes. Proposed mechanisms for shocked PETN chemistry are analyzed as consistent or inconsistent with the data presented here. Our experimental data suggests C≡O or N 2 O bond formation, nitrite formation, and absence of significant hydroxyl or amine concentrations in the initial chemistry steps in PETN shocked above 30 GPa.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A&L Annual Report: GRM-MAPS

Exploding Bridge Wire (EBW) is an important design for initiating detonators relevant to several LLNL systems. In such designs, a metal bridge wire is in direct contact with a porous secondary high explosive (HE), typically pressed to around 50% of its crystalline density. Initiation is believed to occur through shock waves generated when the bridge wire is made to explode via the rapid passing of a strong current pulse. Permeametry is an important characterization tool for the porous powdered HE (PETN, HMX, etc.) component in such devices. Such powders are well known to coarsen with age, with an accompanying deterioration in performance, which includes increased function time and sensitivity. Among various material characteristics, one that has been shown to correlate the most with such performance parameters is the flow-permeable surface area (FSSA), measured using air-permeametry. Commercially available permeametry apparatuses, such as that from Fisher Scientific or a more modern version from Micromeritics suffer from a few drawbacks, most notably as related to monitoring age-related changes in FSSA. This is because it requires re-compaction of the aged powder into the permeametry tube, which in most cases leads to an unwanted increase in FSSA. To address this and a few other shortcomings, we have been developing a modern version of the permeameter, Gee-Reinstein-Maiti Modern Air-Permeametry System (GRM-MAPS). In this report, we summarize progress made in FY25 toward perfecting and calibrating the instrument, which we aim at deploying within surveillance in FY26.

36 MATERIALS SCIENCE↗

An apparatus for the characterization of warm, dense deuterium with inelastic x-ray scattering

Here, we present an instrument platform for studying shock-compressed deuterium on moderately sized laser facilities. The target is designed for cryogenic liquid deuterium to be compressed with a sub-kJ laser pulse. The x-ray probe is the narrow band 2005 eV Si Ly-α resonance produced by a 200J laser incident on a Si 3 N 4 foil. Scattered x-ray collection occurs in the backward and forward directions; spectral dispersion with Bragg crystals yields the plasma conditions of density and temperature. Additionally, the shock is probed with velocity interferometry. Combined with the electron density measurements from forward scattering, this allows average ionization state to be inferred. Proof of principle experiments demonstrate the viability of this technique for studies of the ionization of deuterium along the Hugoniot.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Insight into the chemistry of TNT during shock compression through ultrafast absorption spectroscopies

Thin films of trinitrotoluene (TNT) were shock compressed using the ultrafast laser shock apparatus at Los Alamos National Laboratory. Visible (VIS) and mid-infrared (MIR) transient absorption spectroscopies were simultaneously performed to probe for electronic and vibrational changes during shock compression of TNT. Additionally, three shock pressures (16 GPa, 33 GPa, and 45 GPa) were selected to observe no reaction, incipient reaction, and strongly developed reactions for TNT within the experimental time scale of <250 ps. Negligible absorption changes in MIR or VIS absorptions were observed at 16 GPa. At 33 GPa, MIR absorptions in the 3000 cm -1 –4000 cm -1 range were observed to increase during the shock and continue to increase during the rarefaction, in contrast to the VIS absorption measurements, which increased during the shock and almost fully recovered during rarefaction. At 45 GPa, both VIS and MIR absorptions were strong and irreversible. The intense and spectrally broad MIR absorptions were attributed to short lived intermediates with strong, spectrally broad absorptions that dominate the spectral response. The MIR and VIS absorption changes observed at 33 GPa and 45 GPa were credited to shock induced chemistry, most likely including the formation of a very broad hydrogenic stretch feature. The results from these experiments are consistent with the chemical mechanisms that include O–H or N–H formation such as CH 3 oxidation or C–N homolysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Detonation on a tabletop: Nitromethane with high time and space resolution

Nitromethane (NM), a flammable liquid, has been a model system for the shock-to-detonation transition in homogeneous condensed-phase explosives for over 50 years, but we do not understand the fast processes at the molecular scale in the detonation front at the molecular scale. That is largely because prior studies triggered detonations in bomb-sized charges with input shock durations and times-to detonation that were typically microseconds, which made it impossible to observe the faster processes in real time. Here, we studied NM shocked with 4 ns duration input pulses using a tabletop apparatus with laser-launched flyer plates and arrays of tiny disposable optical cuvettes, where the pressure and temperature were probed in real time (1 ns) with photon Doppler velocimetry, optical pyrometry, and high-speed video. Using a 4 ns shock with an input pressure close to the von Neumann spike pressure of 19 GPa, we achieved the minimum time-to-detonation, about 12 ns, where the time-to-detonation is controlled by fundamental molecular processes. We demonstrated the reproducibility of our detonations and showed that they had the same properties as in bomb-sized charges: our detonation velocity, von Neumann spike and Chapman-Jouguet pressures, temperatures, and reaction zone lengths were the same as in bomb-sized charges. Being able to trigger realistic reproducible detonations from a short pulse makes it possible to investigate molecular and fluid dynamics in the detonation by measuring transient responses in real time. Lastly, we found that it took 6 ns for the temperature to reach 3430 K. The high pressure was observed at about 8 ns, when there was a volume explosion to nearly twice the von Neumann spike pressure before settling down to a steady detonation .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High-Entropy Alloy R&D for Accelerator Beam Window Applications

High-Entropy Alloys are a class of novel material that can offer improved resistance to beam-induced radiation damage and thermal shock. Development of these new alloys to serve as beam windows in multi-megawatt accelerator target applications is ongoing at Fermilab. Currently we are investigating AlCoCrMnTiV alloy systems of 4-6 components for service as beam windows; these compositions are predicted by CALPHAD simulation to have a low density and single-phase BCC crystal structure. The microstructures of these systems are being studied by electron microscopy techniques such as energy dispersive X-ray spectroscopy (EDS) to determine elemental homogeneity and composition, electron backscatter diffraction (EBSD) to quantify grain structure and orientation, and transmission electron microscopy (TEM) to observe defect structures and precipitate formation; nanoindentation is used to probe microstructural mechanical properties. Initial bulk property characterization utilizes differential scanning calorimetry to quantify specific heat capacity (cp), dilatometry to determine the coefficient of thermal expansion (CTE), and time-domain thermoreflectance (TDTR) to measure thermal conductivity (K). A miniature tensile testing apparatus is also being developed to test tensile properties. Post-irradiation examination is currently ongoing for several of these compositions that have been irradiated by low-energy ions to damage levels and at a temperature relevant to beam window applications at future next-generation accelerator facilities. This talk will briefly describe the alloy design and synthesis before going into more depth covering microstructural pre-characterization, and post-irradiation examination results from low-energy ion irradiated specimens. This will be followed by the plans for alloy down selection and future prototypic proton irradiations.

43 PARTICLE ACCELERATORS↗

High-Entropy Alloys for Accelerator Beam Window Applications

Development of novel high-entropy alloys (HEAs) is currently underway for potential use as beam windows in future multi-megawatt target systems at Fermilab. HEAs encompass a new class of materials with a vast design space allowing for material properties to be tailored for particular applications and to potentially offer improved resistance to beam-induced radiation damage and thermal shock effects. The alloy systems being studied consist of several compositions of AlCoCrMnTiV with 4 6 component elements. These alloys are all predicted by CALPHAD simulation to have a single-phase BCC crystal structure and low density, with some compositions displaying ordered, nanoscale precipitates. This presentation will briefly discuss alloy design and synthesis before giving a detailed description of the characterization studies of these HEAs in both the pristine state and post-irradiation by low-energy heavy ions to high damage levels. Electron microscopy techniques to quantify elemental homogeneity and composition, determine grain size, shape, and orientation, and quantify lattice parameters, defect structures and precipitate phases are all being used to study alloy microstructures. Mechanical properties of the alloys at the microscale will be reported. The evolution of these properties as a function of radiation damage will also be described. Bulk thermal characteristics of these HEAs have been tested to measure specific heat capacity and coefficient of thermal expansion as a function of temperature. To determine bulk tensile properties a miniature tensile testing apparatus is under development; it s commissioning will be covered briefly. The talk will conclude with our plans for alloy down-selection.

Burleigh, A. [Fermilab]↗