Publications

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Additive Manufacturing (AM) can create novel and complex engineered material structures. Features such as controlled porosity, micro-fibers and/or nano-particles, transitions in materials and integral robust coatings can be important in developing solutions for fusion subcomponents. A realistic understanding of this capability would be particularly valuable in identifying development paths. Major concerns for using AM processes with lasers or electron beams that melt powder to make refractory parts are the power required and residual stresses arising in fabrication. A related issue is the required combination of lasers or e-beams to continue heating of deposited material (to reduce stresses) and to deposit new material at a reasonable built rate while providing adequate surface finish and resolution for meso-scale features. Some Direct Write processes that can make suitable preforms and be cured to an acceptable density may offer another approach for PFCs.

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We present measurements and modeling of aluminum erosion and redeposition experiments in separate helium and deuterium low power, low density L-mode plasmas at the outer divertor strike point of DIII-D to provide a low-Z material benchmark dataset for tokamak erosion-deposition modeling codes. Coatings of Al ∼100 nm thick were applied to ideal (smooth) and realistic (rough) surfaces and exposed to repeat plasma discharges using the DiMES probe. Redeposition in all cases was primarily in the downstream toroidal field direction, evident from both in-situ spectroscopic and post-mortem non-spectroscopic measurements. The gross Al erosion yield was estimated from film thickness change measurements of small area samples, and was found to be ∼40–70% of the expected erosion yield based on theoretical physical sputtering yields after including sputtering by a 1–3% carbon impurity. The multi-step redeposition and re-erosion process, and hence the measured net erosion yield and material migration patterns, were found to be influenced by the surface roughness and/or porosity. A time-dependent model of material migration accounting for deposit accumulation in hidden areas was developed to reproduce the measurements in these experiments and determine a redeposition probability distribution function for sputtered atoms.

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Additively manufactured (AM) austenitic stainless steels are intriguing candidates for the storage of gaseous hydrogen isotopes because complex vessel geometries can be built more easily than by using conventional machining options. Parts built with AM stainless steel tend to have excellent mechanical properties (with tensile strength, ductility, fatigue crack growth, and fracture toughness comparable to or exceeding that of wrought austenitic stainless steel). However, the solidification microstructures produced by AM processing differ substantially from the microstructures of wrought material. Some features may affect permeability, including some amount of porosity and a greater amount of ferrite. Because the diffusivity of hydrogen in ferrite is greater than in austenite (six orders of magnitude at ambient temperature), care must be taken to retain the performance that is taken for granted due to the base alloy chemistry. Furthermore, AM parts tend to have greater dislocation densities and greater amounts of carbon, nitrogen, and oxygen. These features, along with the austenite/ferrite interfaces, may contribute to greater hydrogen trapping. We report the results of our studies of deuterium transport in various austenitic (304L, 316, and 316L) steels produced by AM. Manufacturing by Powder Bed Fusion (PBF) and two different blown powder methods are considered here (Laser Engineered Net Shaping® (LENS®) and a Direct Laser Powder Deposition (DLPD) method with a higher laser power)). The hydrogen permeability (an equilibrium property) changes negligibly (less than a factor of 2), regardless of chemistry and processing method, when tested between 150 and 500°C. This is despite increases in ferrite content up to FN=2.7. However, AM materials exhibit greater hydrogen isotope trapping, as measured by permeation transients, thermal desorption spectra, and inert gas fusion measurement. The trapping energies are likely modest (<10 kJ/mol), but may indicate a larger population of trap sites than in conventional 300-series stainless steels.

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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.

To address the transport and trapping of hydrogen isotopes, several permeation experiments are being pursued at both Sandia National Laboratories (deuterium gas-driven permeation) and Idaho National Laboratories (tritium gas- and plasma-driven tritium permeation). These experiments are in part a collaboration between the US and Japan to study the performance of tungsten at divertor relevant temperatures (PHENIX). Here we report on the development of a high temperature (≤1150 °C) gas-driven permeation cell and initial measurements of deuterium permeation in several types of tungsten: high purity tungsten foil, ITER-grade tungsten (grains oriented through the membrane), and dispersoid-strengthened ultra-fine grain (UFG) tungsten being developed in the US. Experiments were performed at 500–1000 °C and 0.1–1.0 atm D2 pressure. Permeation through ITER-grade tungsten was similar to earlier W experiments by Frauenfelder (1968–69) and Zaharakov (1973). Data from the UFG alloy indicates marginally higher permeability (< 10×) at lower temperatures, but the permeability converges to that of the ITER tungsten at 1000 °C. The permeation cell uses only ceramic and graphite materials in the hot zone to reduce the possibility for oxidation of the sample membrane. Sealing pressure is applied externally, thereby allowing for elevation of the temperature for brittle membranes above the ductile-to-brittle transition temperature.

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An associated particle neutron generator is described that employs a negative ion source to produce high neutron flux from a small source size. Negative ions produced in an rf-driven plasma source are extracted through a small aperture to form a beam which bombards a positively biased, high voltage target electrode. Electrons co-extracted with the negative ions are removed by a permanent magnet electron filter. The use of negative ions enables high neutron output (100% atomic ion beam), high quality imaging (small neutron source size), and reliable operation (no high voltage breakdowns). The neutron generator can operate in either pulsed or continuous-wave (cw) mode and has been demonstrated to produce 106 D-D n/s (equivalent to ~108 D-T n/s) from a 1 mm-diameter neutron source size to facilitate high fidelity associated particle imaging.

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An understanding of the behavior of hydrogen isotopes in materials is critical to predicting tritium transport in structural metals (at high pressure), estimating tritium losses during production (fission environment), and predicting in-vessel inventory for future fusion devices (plasma driven permeation). Current models often assume equilibrium diffusivity and solubility for a class of materials (e.g. stainless steels or aluminum alloys), neglecting trapping effects or, at best, considering a single population of trapping sites. Permeation and trapping studies of the particular castings and forgings enable greater confidence and reduced margins in the models. For FY15, we have continued our investigation of the role of ferrite in permeation for steels of interest to GTS, through measurements of the duplex steel 2507. We also initiated an investigation of the permeability in work hardened materials, to follow up on earlier observations of unusual permeability in a particular region of 304L forgings. Samples were prepared and characterized for ferrite content and coated with palladium to prevent oxidation. Issues with the poor reproducibility of measurements at low permeability were overcome, although the techniques in use are tedious. Funding through TPBAR and GTS were secured for a research grade quadrupole mass spectrometer (QMS) and replacement turbo pumps, which should improve the fidelity and throughput of measurements in FY16.

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In this work, we examine how deuterium becomes trapped in plasma-exposed tungsten and forms near-surface platelet-shaped precipitates. How these bubbles nucleate and grow, as well as the amount of deuterium trapped within, is crucial for interpreting the experimental database. Here, we use a combined experimental/theoretical approach to provide further insight into the underlying physics. With the Tritium Plasma Experiment, we exposed a series of ITER-grade tungsten samples to high flux D plasmas (up to 1.5 × 1022m-2s-1) at temperatures ranging between 103 and 554 °C. Retention of deuterium trapped in the bulk, assessed through thermal desorption spectrometry, reached a maximum at 230 °C and diminished rapidly thereafter for T > 300 °C. Post-mortem examination of the surfaces revealed non-uniform growth of bubbles ranging in diameter between 1 and 10 μm over the surface with a clear correlation with grain boundaries. Electron back-scattering diffraction maps over a large area of the surface confirmed this dependence; grains containing bubbles were aligned with a preferred slip vector along the <111> directions. Focused ion beam profiles suggest that these bubbles nucleated as platelets at depths of 200 nm-1 μm beneath the surface and grew as a result of expansion of sub-surface cracks. To estimate the amount of deuterium trapped in these defects relative to other sites within the material, we applied a continuum-scale treatment of hydrogen isotope precipitation. In addition, we propose a straightforward model of near-surface platelet expansion that reproduces bubble sizes consistent with our measurements. For the tungsten microstructure considered here, we find that bubbles would only weakly affect migration of D into the material, perhaps explaining why deep trapping was observed in prior studies with plasma-exposed neutron-irradiated specimens. We foresee no insurmountable issues that would prevent the theoretical framework developed here from being extended to a broader range of systems where precipitation of insoluble gases in ion beam or plasma-exposed metals is of interest.

Abstract In this work, we apply low energy ion beam analysis to examine directly how the adsorbed hydrogen concentration and binding configuration on W(1 0 0) depend on temperature. We exposed the tungsten surface to fluxes of both atomic and molecular H and D. We then probed the H isotopes adsorbed along different crystal directions using 1-2 keV Ne⁺ ions. At saturation coverage, H occupies two-fold bridge sites on W(1 0 0) at 25°C. The H coverage dramatically changes the behavior of channeled ions, as does reconstruction of the surface W atoms. For the exposure conditions examined here, we find that surface sites remain populated with H until the surface temperature reaches 200°C. After this point, we observe H rapidly desorbing until only a residual concentration remains at 450°C. Development of an efficient atomistic model that accurately reproduces the experimental ion energy spectra and azimuthal variation of recoiled H is underway.

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Comparisons have been made between heat flux measurements from Langmuir probes and embedded thermocouples in the divertor of DIII-D. Good agreement has been found near the outer strike point (OSP) during L-mode operation with Neutral Beam Injection (NBI) using a sheath power transmission factor (SPTF) of 7, predicted by collisionless 1-D sheath theory. Previous SPTF measurements taken from Langmuir probes and IR imagery on DIII-D demonstrated values below the theoretical limit. The Langmuir probe array has since been upgraded and an embedded thermocouple array has been utilized to measure heat flux. The SPTF has also been measured during a NBI heated H-mode shot. This shot demonstrated a SPTF greater than 7 neat the OSP, which is due to a larger scrape-off layer (SOL) current density during H-mode operation. These studies represent a significant advancement towards finding agreement between theoretical predictions of the SPTF at the divertor and experimental measurements from the divertor diagnostics. © 2013 Published by Elsevier B.V.

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The net erosion of molybdenum by the divertor plasma in the DIII-D tokamak was determined from the reduction in thickness of a thin film test sample after a short exposure to well controlled plasma conditions. The spatial distribution of Mo deposited on adjacent carbon surfaces was also measured. Integration of the total quantity of Mo deposited within 2 cm of the source, gave only 19% of the amount lost from the film indicating that most of the Mo is transported to greater distances, in spite of the short pathlength for ionization of Mo in the divertor plasma. These measurements provide benchmark data for comparisons between gross and net erosion and between measurements and simulations of erosion and deposition, which are discussed in companion papers at this conference. Erosion and deposition of carbon, and deuterium retention were also examined. © 2013 Published by Elsevier B.V.

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Experimental observation of net erosion of molybdenum being significantly reduced compared to gross erosion in the divertor of DIII-D is reported for well-controlled plasma conditions. For the first time, gross erosion rates were measured by both spectroscopic and non-spectroscopic methods. In one experiment a net erosion rate of 0.73 ± 0.03 nm/s was measured using ion beam analysis (IBA) of a 1 cm diameter Mo-coated sample. For a 1 mm diameter Mo sample exposed at the same time the net erosion rate was higher at 1.31 nm/s. For the small sample redeposition is expected to be negligible in comparison with the larger sample yielding a net to gross erosion estimate of 0.56 ± 12%. The gross rate was also measured spectroscopically (386 nm MoI line) giving 2.45 nm/s ± factor 2. The experiment was modeled with the REDEP/WBC erosion/redeposition code package coupled to the ITMC-DYN mixed-material code, with plasma conditions supplied by the OEDGE code using Langmuir probe data input. The code-calculated net/gross ratio is =0.46, in good agreement with experiment. © 2013 Published by Elsevier B.V.

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Chemical vapor deposited (CVD) silicon carbide (SiC) has superior resistance to tritium permeation even after irradiation. Prior work has shown Ultrametfoam to be forgiving when bonded to substrates with large CTE differences. The technical objectives are: (1) Evaluate foams of vanadium, niobium and molybdenum metals and SiC for CTE mitigation between a dense SiC barrier and steel structure; (2) Thermostructural modeling of SiC TPB/Ultramet foam/ferritic steel architecture; (3) Evaluate deuterium permeation of chemical vapor deposited (CVD) SiC; (4) D testing involved construction of a new higher temperature (> 1000 C) permeation testing system and development of improved sealing techniques; (5) Fabricate prototype tube similar to that shown with dimensions of 7cm {theta} and 35cm long; and (6) Tritium and hermeticity testing of prototype tube.

Overview of Plasma Materials Interaction (PMI) activities are: (1) Hydrogen diffusion and trapping in metals - (a) Growth of hydrogen precipitates in tungsten PFCs, (b) Temperature dependence of deuterium retention at displacement damage, (c) D retention in W at elevated temperatures; (2) Permeation - (a) Gas driven permeation results for W/Mo/SiC, (b) Plasma-driven permeation test stand for TPE; and (3) Surface studies - (a) H-sensor development, (b) Adsorption of oxygen and hydrogen on beryllium surfaces.

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In this study, the PISCES-A linear plasma instrument has been used to characterize retention in several carbon fiber composites in order to better understand the factors which lead to elevated retention levels in these materials. The PISCES instrument is capable of subjecting materials to intense fluxes (up to 1022 m-2 s-1) of low energy (150 eV) D+ ions, producing conditions similar to those encountered by plasma facing components in a fusion reactor. In this investigation, three CFCs (fabricated with different manufacturing processes) are compared with the N11 composite used in the Tore Supra reactor. The specific surface areas for these materials were within the range of 0.14-0.55 m2/g. The plasma bombardment conditions were adjusted to provide doses on the order of 1025-1026 m-2 at a sample temperature of 200 °C. After removal from PISCES-A, the amount of D retained in the sample surface was determined via thermal desorption spectroscopy. The measured retention showed a strong correlation with the type of material used and the corresponding BET surface area. By using a CFC with a lower internal porosity, one could expect a reduction in retention by a factor of 5 or more. © 2008 Elsevier B.V.