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At least 73 records · Page 4

Optimization of a Wcl6 CVD System to Coat UO2 Powder with Tungsten

In order to achieve deep space exploration via Nuclear Thermal Propulsion (NTP), Marshall Space Flight Center (MSFC) is developing W-UO2 CERMET fuel elements, with focus on fabrication, testing, and process optimization. A risk of fuel loss is present due to the CTE mismatch between tungsten and UO2 in the W-60vol%UO2 fuel element, leading to high thermal stresses. This fuel loss can be reduced by coating the spherical UO2 particles with tungsten via H2/WCl6 reduction in a fluidized bed CVD system. Since the latest incarnation of the inverted reactor was completed, various minor modifications to the system design were completed, including an inverted frit sublimer. In order to optimize the parameters to achieve the desired tungsten coating thickness, a number of trials using surrogate HfO2 powder were performed. The furnace temperature was varied between 930 C and 1000degC, and the sublimer temperature was varied between 140 C and 200 C. Each trial lasted 73-82 minutes, with one lasting 205 minutes. A total of 13 trials were performed over the course of three months, two of which were re-coatings of previous trials. The powder samples were weighed before and after coating to roughly determine mass gain, and Scanning Electron Microscope (SEM) data was also obtained. Initial mass results indicated that the rate of layer deposition was lower than desired in all of the trials. SEM confirmed that while a uniform coating was obtained, the average coating thickness was 9.1% of the goal. The two re-coating trials did increase the thickness of the tungsten layer, but only to an average 14.3% of the goal. Therefore, the number of CVD runs required to fully coat one batch of material with the current configuration is not feasible for high production rates. Therefore, the system will be modified to operate with a negative pressure environment. This will allow for better gas mixing and more efficient heating of the substrate material, yielding greater tungsten coating per trial.

Belancik, Grace A.

Additive Manufacture of Novel Tungsten Wicking and Heat Transfer Structures

Additive manufacturing (AM) is utilized for fabricating complex geometries from refractory metals, such as tungsten and molybdenum. In this study, plates with ultra-fine and fine lattice structures were manufactured from tungsten to demonstrate printability and the component fabrication advantages of AM. Previous work was completed on individual tungsten lattice structures; this work demonstrates the advantages of printing these structures on tubing and first-wall materials. Initial work using stainless steel demonstrated increased heat transfer properties promoted by these lattice structures. Applications for these structures include wicking structures, heat pipes, and first-wall materials in fusion devices. A major advantage of these designs is the capability to produce a monolithic component with tailored heat transfer and wicking properties. This research helps promote the ability to use liquid lithium in fusion devices since these lattice structures manufactured from tungsten could act as a high temperature first-wall or divertor material and as a wicking structure for liquid lithium. Different lattice structures with varying unit cell sizes and strut thicknesses were printed and the effects of these structures on heat transfer properties were measured. Abrasion resistance of these structures was also investigated. This presentation will discuss the results of these experiments and their implications related to heat transfer applications. This work will help inform the development and implementation of complex geometries made from tungsten for future heat pipe and fusion first-wall or divertor component designs.

Carly J. Romnes

Retention and surface morphology evaluation of fine-grain dispersion-strengthened tungsten for plasma-facing component applications

This study exposed novel fine-grain dispersion-strengthened tungsten (W) to high fluence, low energy deuterium (D) and helium (He) plasmas to evaluate how material microstructure and composition affect hydrogen retention and surface morphology. Tested materials included fine-grain dispersion-strengthened tungsten (DSW) with 3 wt% zirconium carbide (ZrC) dispersoids, fine-grain dense W without any dispersoids (FGW), and coarse-grained polycrystalline ‘ITER-grade’ W. Samples were exposed to D 2 + and He + plasmas at fusion-relevant fluences (∼10 25 m -2 ) and ion energies (75 eV) over a range of temperatures (200 °C, 300 °C, 450 °C for D, 850 °C for He). Helium ion microscopy was performed on the exposed samples to evaluate surface morphology changes and material integrity. After D plasma exposure, the ZrC dispersoids showed near-surface degradation at exposure temperatures above 300 °C, but no detrimental morphology changes were observed for the adjacent W grains. After He plasma-exposure, nano-structured fuzz formation was observed in the tungsten matrix of all samples. The ZrC dispersoids maintained their integrity despite the surrounding fuzz growth, with clear delineation between the W fuzz and dispersoid regions. Thermal desorption spectroscopy showed that ZrC DSW consistently retained more D than the FGW by about a factor of 2 across all temperatures. At 200 °C and 300 °C, the ITER-W displayed lower D retention than both the DSW and FGW, however at 450 °C ITER-W showed the highest retention, about 50% more than DSW. He retention was comparable across all samples, with the highest retention observed in the fine-grain W, only 26% higher than in ITER-W. These insights on retention behavior will inform further optimization of these novel fine-grained tungsten materials with and without dispersoid additives.

Dispersion-strengthened tungsten

Simulations of grain growth in tungsten armor materials under ARC plasma edge operation conditions using an integrated plasma-edge/materials model

An integrated model of grain growth deuterium-exposed tungsten polycrystals, consisting of a two-dimensional vertex dynamics model fitted to atomistic data, has been developed to assess the grain growth kinetics of deuterium-exposed polycrystalline tungsten (W). The model tracks the motion of grain boundaries under the effect of driving forces stemming from grain boundary curvature and differential deuterium concentration accumulation. Here, we apply the model to experimentally synthesized tungsten polycrystals under deuterium-saturated conditions relevant to the ARC concept design. The results indicate rapid grain growth kinetics in the near-surface region adjacent to the plasma, where the temperature reaches 1400 K, whereas the microstructure remains stable deeper in the material with the lower temperature of 1000 K. The combined modeling and analysis further reveal that monolithic tungsten produced via conventional fabrication routes is highly susceptible to grain coarsening at temperatures exceeding 1000 K, largely independent of the magnitude of the applied driving force. Moreover, the accumulation of deuterium near grain boundaries has a pronounced inhibitory effect on grain boundary migration. High-angle grain boundaries ( > 50°) contribute more significantly to the overall grain growth process.

36 MATERIALS SCIENCE

ToF-SIMS spectral analysis of pristine and neutron irradiated single crystal tungsten

Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has many promising features in studying materials including high spatial resolution and high mass accuracy of elements, molecules, and isotopes. Its ability to resolve isotopes is especially attractive in studying transmutation products of single crystal tungsten (SCW) post neutron irradiation. Tungsten (W) is a contender of plasma facing materials (PFMs) due to its high thermal and radiological stability. PFMs to be used in the construction of fusion vessels are subject to high temperature and neutron irradiation, resulting in changes to materials including transmutation, which ultimately impact material mechanical and thermal properties. We used IONTOF TOF.SIMS V instrument equipped with a 30 keV Bi 3 + primary ion beam to study pristine SCW and irradiated SCW speciemens. Scanning electron microscope coupled with focused ion beam (SEM-FIB) was used to reduce the dosage of neutron irradiated tungsten and prepare for specimens for SIMS analysis. Static ToF-SIMS spectra were obtained, and transmutation product peak identification was presented in this work. Identified molecules and molecular fragments were compared against isotope theoretical mass to charge ratios of tungsten, rhenium, osmium, and other relevant products. Our results show that ToF-SIMS provides a viable means to study transmutation products of W post neutron irradiation. Such applications are suitable to investigate transmutation effects on materials that are being considered and developed for fusion pilot plants.

36 MATERIALS SCIENCE

Multi-physics modeling of tungsten collector probe samples during the WEST C4 He campaign

Abstract We describe the results of a multi-scale, multi-physics modeling assessment of SOLPS-ITER, hPIC2, RustBCA and Xolotl, in which five single-crystal tungsten (W) samples were placed in a reciprocating collector probe and exposed to helium (He) plasma in the WEST fusion device. In our models, we considered a pure (100 %) He plasma, as well as one with oxygen (O) present (95% He 5% O) corresponding to the impurity concentration estimated during the C4 He campaign in WEST. Our SOLPS simulations approximately match experimental reciprocating Langmuir probe plasma measurements of plasma density and temperature. Using these plasma parameters as input, hPIC2 and RustBCA predict that the presence of oxygen impurities lead to a 15%–20% decrease in ion and heat fluxes to the surface, and an order of magnitude higher sputtering yields (compared with a pure He plasma). Xolotl predictions for the response of tungsten to plasma surface interactions (PSIs) agree with experimental LAMS analysis, and indicate large near-surface He concentrations, which quickly decay with depth. Our model also shows an increasing role of erosion—in removing the near-surface He—with time. Overall, slightly higher retention is predicted for tungsten exposed to a pure He plasma, with the largest differences in the near-surface gas content caused by the large oxygen-induced erosion. This highlights the important role that impurities play in PSI. Therefore, future work will focus on providing a fully self-consistent description of oxygen (and oxides, etc.) in our models, through multi-species implementation in GITR and inclusion of oxygen and tungsten oxide formation in Xolotl.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY

Gyrokinetic prediction of core tungsten peaking in a WEST plasma with nitrogen impurities

Tungsten peaking is predicted in the core of a WEST plasma with total-f gyrokinetic simulations, including both collisional and turbulent transport. This prediction is validated with a synthetic diagnostic of the bolometry. Although nitrogen impurities are shown to reduce the neoclassical peaking of tungsten on-axis, the overall tungsten peaking increases when nitrogen impurities are present, as they reduce the turbulence screening off-axis. This finding is important for the plasma current ramp-up phase of ITER, where light impurities seeding will be desirable to achieve low temperatures at the plasma-facing components and reduce tungsten sputtering. It provides further argument for applying early ECRH heating to maintain margins on the core power balance. The neoclassical peaking factor is cross-verified between XGC and FACIT. The heat flux at separatrix and the heat load width are modeled by XGC and compared to WEST data.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY

Recrystallization, cracking, and erosion of dispersoid-strengthened tungsten materials during exposure to divertor plasmas

In this study, we investigated the effects of combined intense particle and heat flux exposure on advanced tungsten plasma-facing materials within the DIII-D fusion facility. Our test matrix included two types of dispersoid-strengthened tungsten (containing either 100 nm diameter TiO 2 or Ni particles), along with high-purity polycrystalline tungsten as a reference. This experiment relied on a sample geometry angled at 15° relative to the divertor surface, thereby allowing the surfaces to intercept steady-state perpendicular heat fluxes (q ⟂ ) ranging from 10.1 to 19.6 MW/m 2 . During each shot, the samples were exposed to 42 Hz edge-localized modes (ELMs), allowing us to test the material response to transient heating. We correlated the exposure conditions with extensive post-test surface composition analysis and microscopy to determine how the plasma modified each surface. The angled specimens closest to the strike point received the highest combined heat and particle flux and melted midway through the experiment. EBSD analysis revealed they were completely recrystallized throughout, with an average grain size >100 µm. On the other hand, the specimens that received a lower steady state heat flux survived with more superficial surface damage. Whereas the high-purity polycrystalline tungsten exhibited a higher surface roughness, the dispersoid-strengthened material exhibited more extensive shallow inter-granular cracking. In addition, the surface was depleted of dispersoids following plasma exposure, possibly because of evaporation and/or sputtering. The results described here provide insights into the performance of these materials in a fusion environment which can guide further optimization for use in long-pulse devices.

Kolasinski, Robert D. [Sandia National Laboratorie

Influence of Domain Size and Support Composition on the Reducibility of SiO 2 and TiO 2 Supported Tungsten Oxide Clusters

Supported tungsten oxides are widely used in a variety of catalytic reactions. Depending on the support, the cluster size, oxidation state, reducibility and speciation of the tungsten oxides can widely differ. When promoted with a platinum group metal, the resulting spillover of hydrogen may facilitate the reduction of supported tungsten oxide species, depending on the support. High resolution scanning transmission electron microscopy imaging showed nanometer scale WO x clusters were synthesized on SiO 2 whereas highly dispersed species were formed on TiO 2 . Results from H 2 -temperature-programmed reduction showed the presence of Pd lowered the initial reduction temperature of SiO 2 -supported WO x species but interestingly did not affect that of TiO 2 -supported WO x . X-ray photoelectron and absorption spectroscopies showed the W atoms in SiO 2 -supported WO x species reduce from a +6 oxidation state to primarily +5 after thermal treatment in 5% H 2 , while the fraction of W in the +5 oxidation state was relatively unaffected by reduction treatment of TiO 2 -supported WO x . The unusual behavior of TiO 2 -supported WO x was explained by quantum chemical calculations that reveal the lack of change in the oxidation state of W is attributed to charge delocalization on the surface atoms of the titania support, which does not occur on silica. Moreover, modeling results at <600 K in the presence of H 2 suggest the formation of Brønsted acid sites, and the absence of Lewis acid sites, on larger aggregates of WO x on silica and all cluster sizes on titania. These results provide experimental and theoretical insights into the nature of supported tungsten oxide clusters under conditions relevant to various catalytic reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Elastic constants in monocrystalline tungsten under quasi-hydrostatic pressures to 11.3 GPa

Compressional (P) and shear (S) wave velocities of tungsten single crystals along the [100] and [110] directions were measured using ultrasonic interferometry at room temperature up to 11.3 GPa. Least-squares fitting of $V$$^{[100]}_{P}$, $V$$^{[100]}_{S}$, $V$$^{[110]}_{P}$, and pressure to finite strain (FS) equations yields the elastic constants: C 11 = 523.5(5) GPa, C 12 = 205.1(32) GPa, and C 44 = 160.8(4) GPa, along with their respective pressure derivatives: $C$$^{′}_{11}$ = 6.20(2), $C$$^{′}_{12}$ = 3.35(1), and $C$$^{′}_{44}$ = 1.65(6). Using the Voigt–Reuss–Hill approximation, the elastic moduli were derived as K S0 = 311.2(22) GPa and G 0 = 160.2(7)GPa, along with their respective pressure derivatives: $K$$^{′}_{S0}$ = 4.30(4) and $G$$^{′}_{0}$ = 1.56(1). The Debye temperature of tungsten was determined to be 380.7(8) K, showing good agreement with previous calorimetric measurements. The elastic anisotropy increases slightly from 1.01(1) at ambient pressure to 1.03(1) at 11.3 GPa, suggesting that tungsten remains nearly isotropic under compression. Poisson's ratio slightly increased from 0.281(3) to 0.288(3) with pressure. Additionally, Pugh's ratio decreased from 0.512(4) to 0.494(4), while Pettifor's ratio increased from 0.148(10) to 0.175(10) as pressure reached 11.3 GPa. These results suggest that tungsten is weakly ductile compared to the critical thresholds for ductile behavior (i.e., Pugh's ratio <0.6 and Pettifor's ratio >0, indicating ductile behavior), but that its ductility increases marginally under pressure.

Wang, Ran [Stony Brook University, NY (United Stat

Flash electropolishing for TEM: Reducing FIB‐induced defects in tungsten with protocols for new materials

Focused ion beam (FIB) milling has become the dominant approach for site-specific transmission electron microscopy (TEM) specimen preparation; however, FIB damage remains a critical limitation for reliable microstructural characterisation, particularly in radiation effects studies. Tungsten is especially susceptible to FIB damage due to its high nuclear stopping power, which promotes the formation and strong diffraction contrast of FIB-induced ‘black spot’ defects that are indistinguishable from very fine irradiation-induced loops/defects resulting from low to intermediate temperature neutron irradiation. In this work, flash electropolishing is systematically evaluated as a post-FIB treatment for minimising preparation-induced artefacts for TEM analysis of tungsten-based alloys. Using a range of non-, ion-, and neutron-irradiated tungsten materials, the effectiveness of flash electropolishing has been assessed through direct comparison with conventional FIB and plasma-FIB preparation including low-energy Ga, Ar, Xe ion cleaning. The results demonstrate that flash electropolishing effectively removes FIB-damaged layers and ‘black spot’ defects, thereby enabling reliable observation of irradiation-induced dislocation structures. Key processing parameters governing flash electropolishing quality – including lamella thickness, applied voltage, polishing duration, electrolyte chemistry, and cathode geometry – have been systematically evaluated, and clear criteria were established for determining when flash electropolishing is required to ensure reliable microstructural analysis. This work also provides practical guidance for implementing flash electropolishing as an artefact-controlled specimen-preparation approach for TEM characterisation of FIB-produced specimens. The systematic protocol can be extended to other, non-tungsten materials.

TEM sample preparation

Tungsten wire and tubing joined by nickel brazing

Thin tungsten wire and tungsten tubing are brazed together using a contacting coil of nickel wire heated to its melting point in an inert-gas atmosphere. This method is also effective for brazing tungsten to tungsten-rhenium parts.

Source record

An investigation of the normal momentum transfer for gases on tungsten

The near monoenergetic beam of neutral helium and argon atoms impinged on a single crystal tungsten target, with the (100) face exposed to the beam. The target was mounted on a torsion balance. The rotation of this torsion balance was monitored by an optical lever, and this reading was converted to a measurement of the momentum exchange between the beam and the target. The tungsten target was flashed to a temperature in excess of 2000 C before every clean run, and the vacuum levels in the final chamber were typically between 0.5 and 1 ntorr. The momentum exchange for the helium-tungsten surface and the argon-tungsten surface combination was obtained over approximately a decade of incoming energy (for the argon gas) at angles of incidence of 0, 30, and 41 deg on both clean and dirty (gas covered) surfaces. The results exhibited a significant variation in momentum transfer between the data obtained for the clean and dirty surfaces. The values of normal momentum accommodation coefficient for the clean surface were found to be lower than the values previously reported.

Moskal, E. J.

Fabrication and evaluation of chemically vapor deposited tungsten heat pipe

A network of lithium-filled tungsten heat pipes is considered as a method of heat extraction from high temperature nuclear reactors. The need for material purity and shape versatility in these applications dictates the use of chemically vapor deposited (CVD) tungsten. Adaptability of CVD tungsten to complex heat pipe designs is shown. Deposition and welding techniques are described. Operation of two lithium-filled CVD tungsten heat pipes above 1800 K is discussed.

Bacigalupi, R. J.

Adhesion and transfer of polytetrafluoroethylene to tungsten studied by field ion microscopy

Mechanical contacts between polytetrafluoroethylene (PTFE) and tungsten field ion tips were made in situ in the field ion microscope. Both load and force of adhesion were measured for varying contact times and for clean and contaminated tungsten tips. Strong adhesion between the PTFE and clean tungsten was observed at contact times greater than 2.5 min (forces of adhesion were greater than three times the load). For times less than 2.5 min, the force of adhesion was immeasurably small. The increase in adhesion with contact time after 2.5 min can be attributed to the increase in true contact area by creep of PTFE. No adhesion was measurable at long contact times with contaminated tungsten tips. Neon field ion micrographs taken after the contacts show many linear and branched arrays which appear to represent PTFE that remains adhered to the surface even at the high electric fields required for imaging.

Brainard, W. A.

Fabrication and evaluation of chemically vapor deposited tungsten heat pipe.

A network of lithium-filled tungsten heat pipes is being considered as a method of heat extraction from high temperature nuclear reactors. The need for material purity and shape versatility in these applications dictates the use of chemically vapor deposited (CVD) tungsten. Adaptability of CVD tungsten to complex heat pipe designs is shown. Deposition and welding techniques are described. Operation of two lithium-filled CVD tungsten heat pipes above 1800 K is discussed.

Bacigalupi, R. J.

Fuel Retention Improvement at High Temperatures in Tungsten-Uranium Dioxide Dispersion Fuel Elements by Plasma-Spray Cladding

An investigation was undertaken to determine the feasibility of depositing integrally bonded plasma-sprayed tungsten coatings onto 80-volume-percent tungsten - 20-volume-percent uranium dioxide composites. These composites were face clad with thin tungsten foil to inhibit uranium dioxide loss at elevated temperatures, but loss at the unclad edges was still significant. By preheating the composite substrates to approximately 3700 degrees F in a nitrogen environment, metallurgically bonded tungsten coatings could be obtained directly by plasma spraying. Furthermore, even though these coatings were thin and somewhat porous, they greatly inhibited the loss of uranium dioxide. For example, a specimen that was face clad but had no edge cladding lost 5.8 percent uranium dioxide after 2 hours at 4750 dgrees F in flowing hydrogen. A similar specimen with plasma-spray-coated edges, however, lost only 0.75 percent uranium dioxide under the same testing conditions.

Grisaffe, Salvatore J.

A proposed physical model for the impregnated tungsten cathode based on Auger surface studies of the Ba-O-W system

Auger spectra and work function measurements are used to study the surface reactions between tungsten surface and adsorbed layers of barium, and barium and oxygen. The barium on an impregnated tungsten cathod seems to be an intermediate state, probably a coadsorbed barium-oxygen layer on tungsten. A slightly revised version of the previously suggested (1976) impregnated tungsten cathode model is proposed. This revised model assumes that the cathode surface during life has an adsorbed surface layer of a monolayer or less of both barium and oxygen on the surface. At end of life, steep drop in electron emission and resultant cathode failure occur. Recent NASA life test results on TWT type tubes are reported and explained by the proposed model.

Forman, R.