Publications

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Polymers used in hydrogen transportation, production, storage, and dispensing operations of the hydrogen infrastructure are subject to demanding performance temperatures (-60°C to +140°C) and pressures (0.9 MPa to 87 MPa), under static and cycling conditions of hydrogen exposure. Cycling exposures which include pressurization and depressurization stages can particularly affect properties of these soft materials. Other factors such temperature of exposure in hydrogen environments can also play an influential role on polymer degradation behaviors. In this work, we evaluated the influence of varying rates of depressurization (1, 10, 20, 40 MPa/min and uncontrolled) with model elastomer compounds exposed to high-pressure hydrogen cycling (17 MPa to 87 MPa) at ambient temperature. The goal was to develop an understanding of factors that affect rapid gas decompression in elastomers, which is a phenomenon common in hydrogen fueling operations. Cycling was followed by ex-situ characterization for changes in properties. Dynamic Mechanical Thermal Analysis (DMTA), density, compression set, Attenuated Total Reflectance-FTIR (ATR-FTIR), nanoindentation, and X-ray computer tomography were characterization techniques used to compare polymers before and after cycling. Polymer degradation in the form of internal damage was found to increase with rate of depressurization. EPDM showed the most dependence on rates of depressurization, compared to FKM and HNBR formulations. Additionally, filled, and unfilled model compounds of EPDM, FKM, HNBR, and NBR were tested in high-pressure (17 MPa to 87 MPa) and low-pressure (10 MPa to 31 MPa) cycling conditions at -40°C and +85°C. These experiments were performed at a fixed depressurization rate. The goal of these experiments was to better understand temperature effects under pressure cycling conditions for elastomeric polymer seals. Filled formulations of EPDM, HNBR, and NBR exhibited increased compression set and decreased storage modulus under cold cycling exposures to a greater extent than when cycled at ambient. For filled polymers cycled at low pressures at 85°C and -40°C, FKM showed the most resistance to blistering. HNBR and NBR showed heavy swelling and blistering under both these conditions. Micro CT imaging of one of the polymers (EPDM) subjected to high-pressure cycling at 85°C showed great damage in the form of cracks in the center of the sample. Filled formulations exhibited decreased compression set and storage modulus under hot cycling exposures to a greater extent than with cold and ambient cycling. The findings from these studies will help build a strong understanding of polymer behaviors in cycling hydrogen under rapid gas decompression and thermal conditions encountered in fueling operations and storage. Proper material selection for appropriate use-conditions within components is also enabled.

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Due to challenges in generating high-quality 3D speckle patterns for Digital Volume Correlation (DVC) strain measurements, DVC experiments often utilize the intrinsic texture and contrast of composite microstructures. One common deficiency of these natural speckle patterns is their poor durability under large deformations, which can lead to decorrelation and inaccurate strain measurements. Using syntactic foams as a model material, the effects of speckle pattern degradation on the accuracy of DVC displacement and strain measurements are assessed with both experimentally-acquired and numerically-generated images. It is shown that measurement error can be classified into two regimes as a function of the percentage of markers that have disappeared from the speckle pattern. For minor levels of damage beneath a critical level of damage, displacement and strain error remained near the noise floor of less than 0.05 voxels and 100 με, respectively; above this level, error rapidly increased to unacceptable levels above 0.2 voxels and 10,000 με. This transition occurred after 30%–40% of the speckles disappeared, depending on characteristics of the speckle pattern and its degradation mechanisms. Furthermore, these results suggest that accurate DVC measurements can be obtained in many types of fragile materials despite severe damage to the speckle pattern.

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A sample of natural quartzite rock was submerged in deionized water and illuminated with 1.8-J pulses of 527- nm light with 15-ns duration over an area of 3 cm² [fluence = 0.6 J/cm²]. This relatively low fluence and intensity [40 MW/cm²] were far below the threshold needed for direct ablation via plasma formation or thermal evaporation. With each laser pulse, a small cloud of sub-μm particles was released from the surface and dispersed into the submerging water, forming a long-lived suspension. After one hundred laser pulses, the processing was terminated and the surface of the originally colored quartzite was rendered colorless. The quartzite rock was cut in cross section and the colorless material on the surface was examined with X-ray fluorescence. We report that the transition element Fe was found to be significantly depleted in this colorless layer. This supports the hypothesis that the laser exposure lead to a transient hydrothermal dissolution of the material, followed by a recrystallization process of the SiO₂ that preferentially released iron oxides into the submerging water.

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A simple procedure has been developed to create palladium (Pd) films on the surface of several common polymers used in commercial fused deposition modeling (FDM) and stereolithography (SLA) based three-dimensional (3D) printing by an electroless deposition process. The procedure can be performed at room temperature, with equipment less expensive than many 3D printers, and occurs rapidly enough to achieve full coverage of the film within a few minutes. 3D substrates composed of dense logpile or cubic lattices with part sizes in the mm to cm range, and feature sizes as small as 150 μm were designed and printed using commercially available 3D printers. The deposition procedure was successfully adapted to show full coverage in the lattice substrates. The ability to design, print, and metallize highly ordered three-dimensional microscale structures could accelerate development of a range of optimized chemical and mechanical engineering systems.

In this work, we examine the response of an ultra-fine grained (UFG) tungsten material to high-flux deuterium plasma exposure. UFG tungsten has received considerable interest as a possible plasma-facing material in magnetic confinement fusion devices, in large part because of its improved resistance to neutron damage. However, optimization of the material in this manner may lead to trade-offs in other properties. We address two aspects of the problem in this work: (a) how high-flux plasmas modify the structure of the exposed surface, and (b) how hydrogen isotopes become trapped within the material. The specific UFG tungsten considered here contains 100 nm-width Ti dispersoids (1 wt%) that limit the growth of the W grains to a median size of 960 nm. Metal impurities (Fe, Cr) as well as O were identified within the dispersoids; these species were absent from the W matrix. To simulate relevant particle bombardment conditions, we exposed specimens of the W-Ti material to low energy (100 eV), high-flux (> 1022 m− 2 s− 1) deuterium plasmas in the PISCES-A facility at the University of California, San Diego. To explore different temperature-dependent trapping mechanisms, we considered a range of exposure temperatures between 200 °C and 500 °C. For comparison, we also exposed reference specimens of conventional powder metallurgy warm-rolled and ITER-grade tungsten at 300 °C. Post-mortem focused ion beam profiling and atomic force microscopy of the UFG tungsten revealed no evidence of near-surface bubbles containing high pressure D2 gas, a common surface degradation mechanism associated with plasma exposure. Thermal desorption spectrometry indicated moderately higher trapping of D in the material compared with the reference specimens, though still within the spread of values for different tungsten grades found in the literature database. For the criteria considered here, these results do not indicate any significant obstacles to the potential use of UFG tungsten as a plasma-facing material, although further experimental work is needed to assess material response to transient events and high plasma fluence.

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Thermal desorption spectroscopy was used to monitor the decomposition as a function of temperature for the foam and epoxy as a function of temperature in the range of 60C to 170C. Samples were studied with one day holds at each of the studied temperatures. Both new (FoamN and EpoxyN) and aged (FoamP and EpoxyP) samples were studied. During these ~10 day experiments, the foam samples lost 11 to 13% of their weight and the EpoxyN lost 10% of its weight. The amount of weight lost was difficult to quantify for EpoxyP because of its inert filler. The onset of the appearance of organic degradation products from FoamP began at 110C. Similar products did not appear until 120C for FoamN, suggesting some effect of the previous decades of storage for FoamP. In the case of the epoxies, the corresponding temperatures were 120C for EpoxyP and 110C for EpoxyN. Suggestions for why the aged epoxy seems more stable than newer sample include the possibility of incomplete curing or differences in composition. Recommendation to limit use temperature to 90-100C for both epoxy and foam.

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The equipment and method for and results of calibration of the Sandia/CA TDS system for hydrogen quantification is presented. This technique for calibration can be used to quantify the hydrogen content titanium subhydride, titanium hydride, and any other hydrogen-containing material that desorbs its hydrogen in the form of molecular hydrogen below 1450°C.

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Oxygen gas injection has been studied as one method for rapidly generating hydrogen gas from a uranium hydride storage system. Small scale reactors, 2.9 g UH{sub 3}, were used to study the process experimentally. Complimentary numerical simulations were used to better characterize and understand the strongly coupled chemical and thermal transport processes controlling hydrogen gas liberation. The results indicate that UH{sub 3} and O{sub 2} are sufficiently reactive to enable a well designed system to release gram quantities of hydrogen in {approx} 2 seconds over a broad temperature range. The major system-design challenge appears to be heat management. In addition to the oxidation tests, H/D isotope exchange experiments were performed. The rate limiting step in the overall gas-to-particle exchange process was found to be hydrogen diffusion in the {approx}0.5 {mu}m hydride particles. The experiments generated a set of high quality experimental data; from which effective intra-particle diffusion coefficients can be inferred.

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A prototype of a tritium thermoelectric generator (TTG) is currently being developed at Sandia. In the TTG, a vacuum jacket reduces the amount of heat lost from the high temperature source via convection. However, outgassing presents challenges to maintaining a vacuum for many years. Getters are chemically active substances that scavenge residual gases in a vacuum system. In order to maintain the vacuum jacket at approximately 1.0 x 10{sup -4} torr for decades, nonevaporable getters that can operate from -55 C to 60 C are going to be used. This paper focuses on the hydrogen capacity and absorption rate of the St707{trademark} non-evaporable getter by SAES. Using a getter testing manifold, we have carried out experiments to test these characteristics of the getter over the temperature range of -77 C to 60 C. The results from this study can be used to size the getter appropriately.

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A more reactive liner material is needed for use as liner and cruciform material in tritium producing burnable absorber rods (TPBAR) in commercial light water nuclear reactors (CLWR). The function of these components is to convert any water that is released from the Li-6 enriched lithium aluminate breeder material to oxide and hydrogen that can be gettered, thus minimizing the permeation of tritium into the reactor coolant. Fourteen zirconium alloys were exposed to 2.5 kPa water vapor in a helium stream at 300 C over a period of up to 35 days. Experimental alloys with aluminum, yttrium, vanadium, titanium, and scandium, some of which also included ternaries with nickel, were included along with a high nitrogen impurity alloy and the commercial alloy Zircaloy-2. They displayed a reactivity range of almost 500, with Zircaloy-2 being the least reactive.

In order to determine the visibility of various features by different techniques and in different settings, several test objects containing wires have been used as standards. Examples are shown of the use of x-ray and active thermal imaging for the detection of inclusions. The effect of x-ray accelerating voltage and confounding materials on the x-ray images is shown. Calculated transmission functions for selected materials at a range of voltages are given. The effect of confounding materials, finishes, and textures on thermography is shown and on x-radiography is discussed.

Since sensitivity to contamination is one of the verities of solid state joining, there is a need for assessing contamination of the part(s) to be joined, preferably nondestructively while it can be remedied. As the surfaces that are joined in pinch welds are inaccessible and thus provide a greater challenge, most of the discussion is of the search for the origin and effect of contamination on pinch welding and ways to detect and mitigate it. An example of contamination and the investigation and remediation of such a system is presented. Suggestions are made for techniques for nondestructive evaluation of contamination of surfaces for other solid state welds as well as for pinch welds. Surfaces that have good visual access are amenable to inspection by diffuse reflection infrared Fourier transform (DRIFT) spectroscopy. Although other techniques are useful for specific classes of contaminants (such as hydrocarbons), DRIFT can be used most classes of contaminants. Surfaces such as the interior of open tubes or stems that are to be pinch welded can be inspected using infrared reflection spectroscopy. It must be demonstrated whether or not this tool can detect graphite based contamination, which has been seen in stems. For tubes with one closed end, the technique that should be investigated is emission infrared spectroscopy.

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Power sources capable of supplying tens of watts are needed for a wide variety of applications including portable electronics, sensors, micro aerial vehicles, and mini-robotics systems. The utility of these devices is often limited by the energy and power density capabilities of batteries. A small combustion engine using liquid hydrocarbon fuel could potentially increase both power and energy density by an order of magnitude or more. This report describes initial development work on a meso-scale external combustion engine based on the Stirling cycle. Although other engine designs perform better at macro-scales, we believe the Stirling engine cycle is better suited to small-scale applications. The ideal Stirling cycle requires efficient heat transfer. Consequently, unlike other thermodynamic cycles, the high heat transfer rates that are inherent with miniature devices are an advantage for the Stirling cycle. Furthermore, since the Stirling engine uses external combustion, the combustor and engine can be scaled and optimized semi-independently. Continuous combustion minimizes issues with flame initiation and propagation. It also allows consideration of a variety of techniques to promote combustion that would be difficult in a miniature internal combustion engine. The project included design and fabrication of both the engine and the combustor. Two engine designs were developed. The first used a cylindrical piston design fabricated with conventional machining processes. The second design, based on the Wankel rotor geometry, was fabricated by through-mold electroforming of nickel in SU8 and LIGA micromolds. These technologies provided the requisite precision and tight tolerances needed for efficient micro-engine operation. Electroformed nickel is ideal for micro-engine applications because of its high strength and ductility. A rotary geometry was chosen because its planar geometry was more compatible with the fabrication process. SU8 lithography provided rapid prototypes to verify the design. A final high precision engine was created via LIGA. The micro-combustor was based on an excess enthalpy concept. Development of a micro-combustor included both modeling and experiments. We developed a suite of simulation tools both in support of the design of the prototype combustors, and to investigate more fundamental aspects of combustion at small scales. Issues of heat management and integration with the micro-scale Stirling engine were pursued using CFD simulations. We found that by choice of the operating conditions and channel dimensions energy conversion occurs by catalysis-dominated or catalysis-then-homogeneous phase combustion. The purpose of the experimental effort in micro-combustion was to study the feasibility and explore the design parameters of excess enthalpy combustors. The efforts were guided by the necessity for a practical device that could be implemented in a miniature power generator, or as a stand-alone device used for heat generation. Several devices were fabricated and successfully tested using methane as the fuel.