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At least 109 records · Page 6

Beam Heating of Samples: Modeling and Verification

Energy absorbed from the X-ray beam by the sample requires cooling by forced convection (i.e. cryostream) to minimize temperature increase and the damage caused to the sample by the X-ray heating. In this presentation we will first review the current theoretical models and recent studies in the literature, which predict the sample temperature rise for a given set of beam parameters. It should be noted that a common weakness of these previous studies is that none of them provide actual experimental confirmation. This situation is now remedied in our investigation where the problem of x-ray sample heating is taken up once more. We have theoretically investigated, and at the same time, in addition to the numerical computations, performed experiments to validate the predictions. We have modeled, analyzed and experimentally tested the temperature rise of a 1 mm diameter glass sphere (sample surrogate) exposed to an intense synchrotron X-ray beam, while it is being cooled in a uniform flow of nitrogen gas. The heat transfer, including external convection and internal heat conduction was theoretically modeled using CFD to predict the temperature variation in the sphere during cooling and while it was subjected to an undulator (ID sector 19) X-ray beam at the APS. The surface temperature of the sphere during the X-ray beam heating was measured using the infrared camera measurement technique described in a previous talk. The temperatures from the numerical predictions and experimental measurements are compared and discussed. Additional results are reported for the two different sphere sizes and for two different supporting pin orientations.

Kazmierczak, Michael↗

Shuttle Hypervelocity Impact Database

With three missions outstanding, the Shuttle Hypervelocity Impact Database has nearly 3000 entries. The data is divided into tables for crew module windows, payload bay door radiators and thermal protection system regions, with window impacts compromising just over half the records. In general, the database provides dimensions of hypervelocity impact damage, a component level location (i.e., window number or radiator panel number) and the orbiter mission when the impact occurred. Additional detail on the type of particle that produced the damage site is provided when sampling data and definitive analysis results are available. Details and insights on the contents of the database including examples of descriptive statistics will be provided. Post flight impact damage inspection and sampling techniques that were employed during the different observation campaigns will also be discussed. Potential enhancements to the database structure and availability of the data for other researchers will be addressed in the Future Work section. A related database of returned surfaces from the International Space Station will also be introduced.

Hyde, James L.↗

Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments

We discuss the need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these stressors are combined there may be synergistic effects that enable unique microstructural evolution mechanisms to activate. Understanding of these mechanisms is necessary for the input and refinement of predictive models and critical for engineering of next generation materials. The basic physics and underlying mechanisms require advanced tools to be investigated. The in situ ion irradiation transmission electron microscope (I 3 TEM) is designed to explore these principles. To quantitatively probe the complex dynamic interactions in materials, careful preparation of samples and consideration of experimental design is required. Particular handling or preparation of samples can easily introduce damage or features that obfuscate the measurements. There is no one correct way to prepare a sample; however, many mistakes can be made. The most common errors and things to consider are highlighted within. The I 3 TEM has many adjustable variables and a large potential experimental space, therefore it is best to design experiments with a specific scientific question or questions in mind. Experiments have been performed on large number of sample geometries, material classes, and with many irradiation conditions. The following are a subset of examples that demonstrate unique in situ capabilities utilizing the I 3 TEM. Au nanoparticles prepared by drop casting have been used to investigate the effects of single ion strikes. Au thin films have been used in studies on the effects of multibeam irradiation on microstructure evolution. Zr films have been exposed to irradiation and mechanical tension to examine creep. Ag nanopillars were subjected to simultaneous high temperature, mechanical compression, and ion irradiation to study irradiation induced creep as well. These results impact fields including: structural materials, nuclear energy, energy storage, catalysis, and microelectronics in space environments.

47 OTHER INSTRUMENTATION↗

X-ray Phase Contrast Imaging of the Impact of Multiple HMX Particles in a Polymeric Matrix

The initiation of high explosives (HEs) under shock loading lacks a comprehensive understanding: particularly at the particle scale. One common explanation is the hot spot theory, which suggests that energy in the material resulting from the impact event is localized in a small area causing an increase in temperature that can lead to ignition. This study focuses on the response of HMX particles (a common HE) within a polymer matrix (Sylgard-184 (R)), a simplified example of a polymer-bound explosive (PBX). These PBXs consist of multiple HMX particles in a single polymer-bound sample. A light gas gun was used to load the samples at impact velocities above 400 m/s. The impact events were visualized using X-ray phase-contrast imaging (PCI) allowing real-time observation of the impact event. The experiment used two different types of samples (multi-particle and two crystals) and found evidence of cracking and debonding in both sample types. Additionally, it was found that the multiple particle samples showed similar evidence of damage at lower velocities than that of single particle samples. This is an expected result as the multiple particles add additional interfaces for stress concentration and frictional heating.

42 ENGINEERING↗

Shuttle Hypervelocity Impact Database

With three flights remaining on the manifest, the shuttle impact hypervelocity database has over 2800 entries. The data is currently divided into tables for crew module windows, payload bay door radiators and thermal protection system regions, with window impacts compromising just over half the records. In general, the database provides dimensions of hypervelocity impact damage, a component level location (i.e., window number or radiator panel number) and the orbiter mission when the impact occurred. Additional detail on the type of particle that produced the damage site is provided when sampling data and definitive analysis results are available. The paper will provide details and insights on the contents of the database including examples of descriptive statistics using the impact data. A discussion of post flight impact damage inspection and sampling techniques that were employed during the different observation campaigns will be presented. Future work to be discussed will be possible enhancements to the database structure and availability of the data for other researchers. A related database of ISS returned surfaces that are under development will also be introduced.

Hyde, James I.↗

Plasma Interactions with a Negative Biased Electrodynamic Tether

The ProSEDS conductive tether design incorporates two distinct types of tethers from a plasma interaction viewpoint. The 200 m closest to the Delta 11 spacecraft is insulated from the plasma, and the remaining 5000 m is semi-bare. This latter portion is semi-bare because it has a conductive coating applied to the wires to permit electron collection while also regulating the overall tether temperature. Because the tether possesses these two distinct types of tethers, a transition point exists between the two types that form a triple point with the space plasma. Insulated tethers can suffer from a second plasma interaction if the insulation is weakened or breached, such as by pinholes caused by small particle debris strikes. Because electrodynamic tethers are typically long, they have a high probability of such impacts. These impacting particles may not be of sufficient size to severe the tether, but they can easily be of sufficient size to damage the tether insulation. Samples of both the ProSEDS tether transition region and the insulated tether section (with various degrees of pinhole damage) were placed into the MSFC plasma chamber and biased to typical ProSEDS open circuit tether potentials (-500 V to -1600 V). The results of the testing showed that the transition region of the tether (i.e. the triple point) arced and burned the tether in two at -900 V, and the damaged insulated sections arced and burned in two between -1000 V and -1600, depending on the pinhole damage geometry. tether design and make the tether ready for flight. To reduce the pinhole arcing risk, ProSEDS mission operations were changed to eliminate the negative potential on the tether. The results of the testing campaign and the design changes implemented to ensure a successful flight will be described.

Vaughn, Jason A.↗

Lamb Wave Assessment of Fatigue and Thermal Damage in Composites

Among the various techniques available, ultrasonic Lamb waves offer a convenient method of evaluating composite materials. Since the Lamb wave velocity depends on the elastic properties of a structure, an effective tool exists to monitor damage in composites by measuring the velocity of these waves. Lamb wave measurements can propagate over long distances and are sensitive to the desired in-plane elastic properties of the material. This paper describes two studies which monitor fatigue damage and two studies which monitor thermal damage in composites using Lamb waves. In the fatigue studies, the Lamb wave velocity is compared to modulus measurements obtained using strain gage measurements in the first experiment and the velocity is monitored along with the crack density in the second. In the thermal damage studies, one examines samples which were exposed to varying temperatures for a three minute duration and the second includes rapid thermal damage in composites by intense laser beams. In all studies, the Lamb wave velocity is demonstrated to be an excellent method to monitor damage in composites.

Seale, Michael D.↗

TRISO PARTICLE FUEL POLISHING PROCESS COMPARISON

The investigation of the TRISO coated particles is important in terms of verification the quality of the nuclear fuel samples before placing them in the reactor core. To determine the degree of damage to the coated particles, the samples must be properly polished in order to uncover the inner layers. The poster presents a comparison of two polishing methods. Mechanical polishing method, which is used frequently for sample preparations generates additional mechanical damages in the studied fuel particle, thus directly affecting the experimental results. Due to that, a novel way to polish the samples is presented - an ionic polishing method. Based on the obtained results, it was concluded that the ion polishing method is better because the level of interference with the structures of the individual layers of the tested samples is much lower than with the mechanical method.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microfluidic liquid sheets as large-area targets for high repetition XFELs

The high intensity of X-ray free electron lasers (XFELs) can damage solution-phase samples on every scale, ranging from the molecular or electronic structure of a sample to the macroscopic structure of a liquid microjet. By using a large surface area liquid sheet microjet as a sample target instead of a standard cylindrical microjet, the incident X-ray spot size can be increased such that the incident intensity falls below the damage threshold. This capability is becoming particularly important for high repetition rate XFELs, where destroying a target with each pulse would require prohibitively large volumes of sample. We present here a study of microfluidic liquid sheet dimensions as a function of liquid flow rate. Sheet lengths, widths and thickness gradients are shown for three styles of nozzles fabricated from isotropically etched glass. In-vacuum operation and sample recirculation using these nozzles is demonstrated. The effects of intense XFEL pulses on the structure of a liquid sheet are also briefly examined.

47 OTHER INSTRUMENTATION↗

Method for Estimating Thread Strength Reduction of Damaged Parent Holes with Inserts

During normal assembly and disassembly of bolted-joint components, thread damage and/or deformation may occur. If threads are overloaded, thread damage/deformation can also be anticipated. Typical inspection techniques (e.g. using GO-NO GO gages) may not provide adequate visibility of the extent of thread damage. More detailed inspection techniques have provided actual pitch-diameter profiles of damaged-hardware holes. A method to predict the reduction in thread shear-out capacity of damaged threaded holes has been developed. This method was based on testing and analytical modeling. Test samples were machined to simulate damaged holes in the hardware of interest. Test samples containing pristine parent-holes were also manufactured from the same bar-stock material to provide baseline results for comparison purposes. After the particular parent-hole thread profile was machined into each sample a helical insert was installed into the threaded hole. These samples were tested in a specially designed fixture to determine the maximum load required to shear out the parent threads. It was determined from the pristine-hole samples that, for the specific material tested, each individual thread could resist an average load of 3980 pounds. The shear-out loads of the holes having modified pitch diameters were compared to the ultimate loads of the specimens with pristine holes. An equivalent number of missing helical coil threads was then determined based on the ratio of shear-out loads for each thread configuration. These data were compared with the results from a finite element model (FEM). The model gave insights into the ability of the thread loads to redistribute for both pristine and simulated damage configurations. In this case, it was determined that the overall potential reduction in thread load-carrying capability in the hardware of interest was equal to having up to three fewer threads in the hole that bolt threads could engage. One- half of this potential reduction was due to local pitch-diameter variations and the other half was due to overall pitch-diameter enlargement beyond Class 2 fit. This result was important in that the thread shear capacity for this particular hardware design was the limiting structural capability. The details of the method development, including the supporting testing, data reduction and analytical model results comparison will be discussed hereafter.

Johnson, David L.↗

Thermal shock resistance of lightweight cements developed for geothermal conditions

Cements are a critical component in well construction, as they act to prevent well fluid and gas escape, prevent corrosion of the casing, and strengthen the wellbore to prevent deformation. Under the high temperature/pressure conditions common in geothermal systems, the injection of cold water for energy production is expected to induce cyclic damage to the borehole cement through the rapid temperature fluctuations. These “thermal shocks” are expected to cause casing shrinkage, annulus formation, and cement tensile stresses. To understand the effect of cold water injection on the wellbore environment, a set of rock-cement-steel samples were created to simulate the structure of a geothermal well. Lightweight thermally-insulating cement blends were tested under thermal shock conditions in this study. In each test, the samples were pressurized to an effective pressure of ~3.5 MPa and placed at high temperatures. Thermal shocks were performed by injecting cold water (~10-15 °C) through the samples at a constant rate while keeping the samples at high temperatures until the sample temperature stopped decreasing and deformation ceased. Eight thermal shock tests were conducted with each sample – two at 100 °C and six at 200 °C. Post-tests analysis was then conducted by cutting open each sample to examine the damage in each component of the simulated wellbore. Experimental results suggest that all samples experienced similar degrees of axial and lateral contraction during cold water injection, but for the most part this contraction is recoverable when injection halts. Post-test analysis revealed that fly ash cenosphere pre-treatment had the best effect on improving thermal shock resistance in the cement blends. Thermomechanical modeling of likely stress paths experienced by the cements during heating/cooling cycles shows that elasto-plastic cement constitutive behavior results in most plastic strain occurring during the initial heating steps, with mostly elastic strain occurring during the thermal shock cycles. In conclusion, this agrees with experimental evidence, suggesting that cement damage from shocking occurs via other mechanisms such as chemical alteration, corrosion, and fatigue.

36 MATERIALS SCIENCE↗

Simulated Space Environment Effects on a Candidate Solar Sail Material

For long duration missions of solar sail vehicles, the sail material needs to survive the harsh space environment as the degradation of the sail material determines its operational lifetime. Therefore, understanding the effects of the space environment on the sail membrane is essential for mission success. In this study, the effect of simulated space environments of ionizing radiation and thermal aging were investigated. In order to assess some of the potential damage effects on the mechanical, thermal and optical properties of a commercial off the shelf (COTS) polyester solar sail membrane. The solar sail membrane was exposed to high energy electrons [about 70 keV and 10 nA/cm(exp. 2)], and the physical properties were characterized. After about 8.3 Grad dose, the tensile modulus, tensile strength and failure strain of the sail membrane decreased by 20 to 95%. The aluminum reflective layer was damaged and partially delaminated but it did not show any significant change in solar absorbance or thermal emittance. The mechanical properties of a precracked sample, simulating potential impact damage of the sail membrane, as well as thermal aging effects on metallized PEN (polyethylene naphthalate) film, will be discussed.

Kang, Jin Ho↗

In-situ Characterizations of Microstructural Degradation of Perovskite Solar Cells

Rapid progress has been achieved in perovskite solar cells (PSCs), and their efficiencies have improved from 3.8 % to 24.2 % in less than a decade. With low-cost processing, PSCs have shown exciting photovoltaic (PV) properties, such as effective optical absorption, a long carrier lifetime, and unique defect tolerance. While recent studies demonstrated improved stability up to 100 days, PSC technology is still challenged to meet the stringent industry requirements for commercialization. Despite considerable efforts, the underlying physical mechanisms for the inferior stability of PSCs are not well understood. One reason for this divergence is that many established measurement techniques (e.g., quantum efficiency, photoluminescence) probe the properties on length scales far greater than that of electronic and/or structural inhomogeneity (i.e., < 1 μm near grain boundaries) and therefore characterize convoluted and/or averaged properties. Ion/electron beam-based techniques have been extensively used to access the microstructures of PSCs, enabling atomic/nanoscale structural, chemical, optical, and electrical characterizations. For example, focused ion beam (FIB) milling produces an atomically smooth surface that minimizes the artifacts attributed to the surface roughness. FIB techniques can also create a well-defined cross-section of PSCs without mechanical damage in a physical cleaving sample preparation. While powerful, there are some concerns about possible beam damage of inorganic-organic perovskites via chemical-bond breakage and local heating. This project aims to comprehensively understand how the microstructural/interfacial properties of PSCs (e.g., Methylammonium Lead Iodide [MAPbI 3 ]) are modified under the irradiating ion beams. Specifically, we investigate the sub-surface properties of PSCs before and after Ar-ion beam injections. Kelvin probe force microscopy (KPFM) measures the contact potential differences (CPDs). Photoluminescence (PL) microscopy in conjunction with Finite-Difference Time-Domain (FDTD) simulations infers the formation of a “dead layer” (< 15 nm) on the subsurface of MAPbI 3 during Ar+ milling processes while preserving the initial bulk properties. The x-ray photoemission spectroscopy (XPS) confirms this modified surface is a lead-rich and iodine-deficient surface. We initiate customizing in-situ measurement setup while measuring the local optical and electrical properties of PSC under thermal (cooling, heating) and light stressors. Our results provide in-depth knowledge of the ion-beam impact on metal-halide perovskites and how this modified sub-surface impacts their properties under accelerated stressors of light and heat. Intensive Monte Carlo simulations of an electron beam interacting with PSCs provide the beam energy distribution in PSCs, proposing possible measurement conditions of using e-beam with minimizing beam damage. Our in-situ measurement platform can accommodate the diverse architecture of PSC devices for studying deterioration mechanisms under mixed environmental stressors.

14 SOLAR ENERGY↗

Effect of rhenium addition on deuterium retention in neutron-irradiated tungsten

In this work, the effects of rhenium (Re) addition on deuterium (D) retention in neutron-irradiated tungsten (W) were investigated. Pure W and W-5Re (5 at.%) alloy samples were irradiated with neutrons at High Flux Isotope Reactor using MFE-RB-19 J capsule. The sample temperature and the damage level were 864 K and 0.35 dpa for pure W and 792 K and 0.26 dpa for W-5Re alloy. A portion of the samples was exposed to D plasma at Tritium Plasma Experiment at Idaho National Laboratory at 823 K to a fluence of 5 × 1025 m -2 . Vacancy-type defects in neutron-irradiated samples were examined using positron annihilation spectroscopy (PAS); D retention after plasma exposure was evaluated by thermal desorption spectrometry (TDS). TDS measurements revealed that D retention in the neutron-irradiated W-5Re alloy was similar to that in the unirradiated W sample, whereas a significant increase in D retention was observed in neutron-irradiated W. Thus, Re addition significantly suppressed the increase in D retention after neutron irradiation. This effect was attributed to the suppression of vacancy-type defect formation, as confirmed by PAS.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

The NASA, Marshall Space Flight Center drop tube user's manual

A comprehensive description of the structural and instrumentation hardware and the experimental capabilities of the 105-meter Marshall Space Flight Center Drop Tube Facility is given. This document is to serve as a guide to the investigator who wishes to perform materials processing experiments in the Drop Tube. Particular attention is given to the Tube's hardware to which an investigator must interface to perform experiments. This hardware consists of the permanent structural hardware (with such items as vacuum flanges), and the experimental hardware (with the furnaces and the sample insertion devices). Two furnaces, an electron-beam and an electromagnetic levitator, are currently used to melt metallic samples in a process environment that can range from 10(exp -6) Torr to 1 atmosphere. Details of these furnaces, the processing environment gases/vacuum, the electrical power, and data acquisition capabilities are specified to allow an investigator to design his/her experiment to maximize successful results and to reduce experimental setup time on the Tube. Various devices used to catch samples while inflicting minimum damage and to enhance turnaround time between experiments are described. Enough information is provided to allow an investigator who wishes to build his/her own furnace or sample catch devices to easily interface it to the Tube. The experimental instrumentation and data acquisition systems used to perform pre-drop and in-flight measurements of the melting and solidification process are also detailed. Typical experimental results are presented as an indicator of the type of data that is provided by the Drop Tube Facility. A summary bibliography of past Drop Tube experiments is provided, and an appendix explaining the noncontact temperature determination of free-falling drops is provided. This document is to be revised occasionally as improvements to the Facility are made and as the summary bibliography grows.

Rathz, Thomas J.↗

ARC-DPA 1-MeV Neutron Fluence Equivalence Model for GaAs

Here, the legacy data used in the production of the American Society for Testing and Materials (ASTM) E722 standard for gallium arsenide (GaAs) were fit with the athermal recombination corrected-displacements per atom (ARC-DPA) model for the development of a novel 1-MeV neutron equivalent fluence metric. Improving on previous work, the coefficients for the ARC-DPA model were optimized using a conjugate gradient method, and the uncertainties in the observed damage in different benchmark neutron fields were sampled to quantify their contribution to the damage metric. The optimized parameters of −0.474 ± 0.03 for b arcdpa and 0.016 ± 0.002 for c arcdpa provided good agreement and indicated that the solution is not sensitive to the corresponding fluence uncertainties. Compared to the current 1-MeV neutron fluence equivalence standard for displacement damage in GaAs, our results indicate that for a thermal reactor neutron environment, displacement damage has been underestimated by around 25% and that the saturation value for the damage efficiency had been higher than previously modeled.

1-MeV equivalent fluence↗

Proton radiation damage in optical filter glass

Samples of Schott BG-39 and Hoya CM-500 blue-green filter glass were subjected to proton radiation to determine their acceptability for spaceflight. Initial testing done with 2.7 MeV protons showed negligible change in optical transmittance with doses as high as 5.2 x 10 to the 14th protons per sq cm. Irradiation with protons of energy up to 63 MeV caused a significant reduction in transmittance in the Schott samples at doses of 5.3 x 10 to the 12th protons per sq cm, while negligible change occurred in the Hoya samples.

Grillot, Patrick N.↗

Simulated Space Environment Effects on a Candidate Solar Sail Material

For long duration missions of solar sails, the sail material needs to survive harsh space environments and the degradation of the sail material controls operational lifetime. Therefore, understanding the effects of the space environment on the sail membrane is essential for mission success. In this study, we investigated the effect of simulated space environment effects of ionizing radiation, thermal aging and simulated potential damage on mechanical, thermal and optical properties of a commercial off the shelf (COTS) polyester solar sail membrane to assess the degradation mechanisms on a feasible solar sail. The solar sail membrane was exposed to high energy electrons (about 70 keV and 10 nA/cm2), and the physical properties were characterized. After about 8.3 Grad dose, the tensile modulus, tensile strength and failure strain of the sail membrane decreased by about 20 ~ 95%. The aluminum reflective layer was damaged and partially delaminated but it did not show any significant change in solar absorbance or thermal emittance. The effect on mechanical properties of a pre-cracked sample, simulating potential impact damage of the sail membrane, as well as thermal aging effects on metallized PEN (polyethylene naphthalate) film will be discussed.

Kang, Jin Ho↗