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At least 19 records

The dependence of tungsten fuzz layer thickness and porosity on tungsten deposition rate and helium ion fluence

Abstract Fuzz formation on a heated tungsten surface in the presence of a helium-containing plasma and tungsten deposition source was investigated. Tungsten samples were exposed at 1123 K to pure helium plasma with ion incident energy of 76 eV, W/He ion flux ratio of ∼ 0.4 × 10 − 4 , and varied helium ion fluence from 0.18 to 3.4 × 10 26 m −2 . Fuzz thickness was measured by cross-sectional scanning electron microscopy to increase from 0.22 to 15 µ m with increasing helium ion fluence. No indication of saturation in fuzz thickness at high fluence was observed, in contrast to fuzz produced on a tungsten surface without tungsten deposition. Additional tungsten samples were exposed at 1123 K to pure helium plasma with ion incident energy of 76 eV, helium ion fluence of ∼ 3.4 × 10 26 m −2 , and varied W/He ion flux ratio from 0.26 to 3.0 × 10 − 4 . Fuzz thickness increased from 7.5 to 120 µ m with increasing W/He ion ratio. A final sample exposed at 1123 K to a mixed helium-deuterium plasma with ion incident energy of 76 eV, helium ion fluence of 0.18 × 10 26 m −2 , and W/He ion flux ratio of 2.2 × 10 − 4 developed nearly identical fuzz structures to that developed in a pure He plasma. As a function of deposited tungsten fluence, all results were found to trace out a single layer-growth curve given by a power law relation, indicating that fuzz thickness is independent of the W/He ion flux ratio in the range investigated and independent of any deuterium present in the plasma. As a result, for tungsten plasma facing walls in magnetic fusion devices at 1000–2000 K with 10 −4 W/He ion flux ratio, fuzz with thicknesses greater than hundreds of microns may form in as little as 10 4 s (in the absence of ELM-induced erosion or annealing), and may more significantly affect its thermophysical properties than fuzz generated without a tungsten deposition source.

Physics↗

Tungsten erosion and divertor leakage from the DIII-D SAS-VW tungsten-coated divertor in experiments with neon gas seeding

Collector probes have been used to examine tungsten divertor leakage in a variety of scenarios with low-Z impurity seeding during operation with the new tungsten-coated SAS-VW divertor in DIII-D. Measurements of tungsten deposition on collector probes inserted into the far Scrape-off-Layer (SOL) are used to deduce how efficiently tungsten leaks out of the closed, V-shaped divertor after it is eroded from the target surfaces. Qualitative differences in the tungsten deposition patterns across the collector probes provide clear experimental evidence that the SOL conditions depend on the low-Z impurity seeding conditions. These measurements show that in scenarios where neon gas is injected into the plasma, the tungsten divertor leakage and SOL transport depend on the poloidal location from which the neon is injected. In particular, neon injection from the Inner Midplane and Outer Midplane appear to each result in higher divertor leakage by a factor of 2 to 3 compared to cases with neon injection from either the SOL Crown or from the SAS-VW divertor itself.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Direct Observation of Tungsten Oxidation Studied by In Situ Environmental TEM

In this study, in situ environmental transmission electron microscopy (ETEM) was applied, for the first time, to investigate the thermal oxidation of a pristine and a self-ion irradiated polycrystalline tungsten, using a MEMS-based gas cell at 500 oC to 900 oC in a 1 bar 2%O2/N2 gas mixture. By tracking the dynamic evolution of the tungsten oxide scale as it initiates, grows, and sublimates during a consecutive thermal oxidation experiment, we observed two distinctive tungsten oxide microstructure – one nanocrystalline o-WO3 scale grown on W{27-1 } and W{1-1 8} and another o-WO3 scale exhibits a novel highly textured nanostructure. While the two oxide microstructures shared a similar thickness of ~200 nm after 40-minute early-stage oxidation, the nanocrystalline scale on the W{27-1 } grew much more rapidly at 800 oC than the highly textured oxide at a higher temperature of 900 oC. This suggests both the microstructure of these tungsten oxide scales as well as their oxidation kinetics are highly sensitive to the tungsten surface orientation, and such correlations also change dynamically in the course of oxidation. We also discuss the tungsten oxidation mechanism, the effects of the TEM foil thickness, and the focused ion beam (FIB) Ga+ damage on in situ ETEM oxidation.

In situ ETEM, Tungsten, Thermal oxidation, Orienta↗

In-Situ Helium Implantation and TEM Investigation of Radiation Tolerance to Helium Bubble Damage in Equiaxed Nanocrystalline Tungsten and Ultrafine Tungsten-TiC Alloy

The use of ultrafine and nanocrystalline materials is a proposed pathway to mitigate irradiation damage in nuclear fusion components. Here, we examine the radiation tolerance of helium bubble formation in 85 nm (average grain size) nanocrystalline-equiaxed-grained tungsten and an ultrafine tungsten-TiC alloy under extreme low energy helium implantation at 1223 K via in-situ transmission electron microscope (TEM). Helium bubble damage evolution in terms of number density, size, and total volume contribution to grain matrices has been determined as a function of He+ implantation fluence. The outputs were compared to previously published results on severe plastically deformed (SPD) tungsten implanted under the same conditions. Large helium bubbles were formed on the grain boundaries and helium bubble damage evolution profiles are shown to differ among the different materials with less overall damage in the nanocrystalline tungsten. Compared to previous works, the results in this work indicate that the nanocrystalline tungsten should possess a fuzz formation threshold more than one order of magnitude higher than coarse-grained tungsten.

36 MATERIALS SCIENCE↗

The effect of high-power transient events on tungsten and tungsten coatings used for radio frequency launcher applications

High-temperature plasma-facing material coatings used for radio frequency (RF) launchers need to be robust enough to survive RF breakdown arcing or other transient events from the plasma (e.g., an edge localized mode) without causing a catastrophic failure of the coating. High-power transient effects are being explored by using an RF-induced vacuum arc to determine the robustness of tungsten coatings made by a variety of manufacturing methods. A 1/4-wavelength resonant section of vacuum transmission line terminated with an open circuit electrode structure with a well-defined electric field (30-60 kV/mm) produces repeatable arcing conditions. The initial focus is on tungsten as a plasma-facing material, including sintered tungsten, tungsten coatings on steel produced via physical vapor deposition (PVD), and functionally graded tungsten/steel coatings deposited by low-pressure plasma-spraying (LPPS). Thin PVD coatings (1-2 microns) fail catastrophically from an arc and result in severe delamination of the coating. The arc-induced damage of thicker coatings, such as those made via LPPS, tend to be restricted to the top few microns of the surface. Arcing often initiates on sharp surface microstructures and causes localized melting of tungsten at the surface of all the materials studied and results in resolidified melt pools with surface cracks. The resolidified surface results in a reduction in overall deuterium retention when exposed to typical RF plasma sheath conditions.

Caughman, John [ORNL] (ORCID:0000000206091164)↗

Diffusion bonding of tungsten-vanadium-zirconium using vacuum hot pressing for the development of a low decay heat cladding solution for tungsten spallation targets

Tantalum has been used as cladding material for water-cooled solid tungsten targets at many leading spallation neutron production facilities thanks to its high neutron yield, manageable radiation damage behavior, and excellent corrosion/erosion resistance in radiation environments. However, from a safety hazard perspective, thermal neutron capture of tantalum in spallation environments causes a high specific decay heat in the target volume, which often becomes a limiting factor in increasing the beam power on the target. In this paper, we studied vacuum hot pressing (VHP) parameters to diffusion bond zirconium to tungsten to explore the feasibility of using zirconium alloys as an alternative cladding material to tantalum. Zirconium alloys have long been used as cladding material for early generation solid spallation targets, and nuclear fuel rods. In spallation environments zirconium has significantly lower decay heat with shorter decay time compared to tantalum. The hot isostatic pressing (HIP) of zirconium and tungsten is known to produce limited bonding quality due to the formation of the brittle ZrW2 intermetallic layer. To overcome this problem, placing a vanadium interlayer between tungsten and zirconium has been proposed by exploring parameter space in binary alloy phase diagrams. Under the VHP conditions, 860 ◦C at 70 MPa for 4 hours, Zr-V and V-W showed good diffusion bonding, which demonstrates the feasibility of a single step HIP process to make the zirconium alloy clad tungsten spallation volumes.

Lee, Yong Joong↗

Thermal diffusivity of irradiated tungsten and tungsten-rhenium alloys

The Japan-US PHENIX project irradiated tungsten materials in the RB-19J capsule experiment in the High Flux Isotope Reactor (HFIR). A gadolinium (Gd) shielding was used to absorb the thermal neutrons and reduce rhenium and osmium generation in tungsten. Pure tungsten and K-doped W-3% Re samples were irradiated at 532 – 662 °C to dose of 0.21-0.46 dpa, with the grain orientation perpendicular or parallel to the disk surface. Thermal diffusivity measurements were performed from 100 °C to 500 °C. Furthermore, additional measurements followed after annealing up to 900 °C. Irradiated pure tungsten specimens showed similar thermal diffusivity results compared with an unirradiated W-1% Re specimen in another study. The transmutation amount of Re was calculated to be about 0.52% for those specimens that showed good agreement with this study. Specimens irradiated in this study to different doses presented almost the same thermal diffusivity. Annealing up to 800 °C resulted in no recovery of thermal diffusivity. These results show that the contribution of crystalline defects to degradation of thermal diffusivity is quite limited. In addition, the thermal diffusivity of the irradiated specimens was getting close to that of the unirradiated specimens at elevated temperature.

36 MATERIALS SCIENCE↗

A review on additive manufacturing of refractory tungsten and tungsten alloys

Here we review the progress of additive manufacturing effort on refractory metal tungsten and tungsten alloys. These materials are excellent candidates for a variety of high temperature applications but extremely challenging to fabricate via additive manufacturing due to a series of existing issues during the manufacturing. We outline these issues and discuss the current understanding and progress to tackle them. Laser powder-bed-fusion, laser directed-energy-deposition, and electron beam powder-bed-fusion are three common techniques that have been applied to additively manufacture pure tungsten. This overview discusses current observations and understanding on the issues associated with each of these techniques. We identify future research opportunities in additive manufacturing of refractory metals.

36 MATERIALS SCIENCE↗

Intense cyclic heating effects on thermo-fracture and thermal shock of solid tungsten and open-cell tungsten foam

Here we investigate here the effects of transient (cyclic) arc-jet plasma and laser heating on fracture behavior of W-foam and solid tungsten. The two key parameters that control the foam thermomechanical response are its density and mean cell size expressed in Pores Per Inch (PPI). Tungsten foam samples were fabricated with Chemical Vapor Deposition (CVD) with variety of PPI and relative density. These were tested under two types of qualitatively different conditions: (1) high-enthalpy arc-jet, and (2) high-power cyclic laser heating. None of the foam samples showed macroscopic through-thickness cracks. However, distributed micro-cracks were observed on ligaments and their triple junctions. Under the same loading conditions, W-foam and solid tungsten showed similar crack network pattern and characteristic length-scale. However, Crack Opening Displacement (COD) was twice as large in solid W as compared to W-foam. Foam samples that have been previously exposed to a low-pressure helium plasma showed significant changes in their surface forming nano-texture fuzz which was removed by subsequent testing in the arc-jet. Extensive fracture and re-crystallization were observed in the thin solid W disk that was fully-constrained from expansion. Thicker and fully-constrained solid W disks did not display recrystallization, grain growth, and extensive cracking. However, thicker disks that were free to expand showed some recrystallization and extensive through-thickness cracks due to less effective cooling and thus higher temperatures. Laser beam testing showed no visible damage formation at 0.19 GW/m 2 and 0.38 GW/m 2 for both low-density (23%) and high-density (43%) foams at low pulses (100-1000). Micro-cracks were observed after 10,000 pulses at 0.19 GW/m 2 in both foams, and in low-density foam after 100,000 at 0.38 GW/m 2 . The nature of thermomechanical damage in W-foam exposed to extreme power (GW/m 2 ) short-duration laser pulses was found to be qualitatively similar to that of high power (MW/m 2 ) long-duration arc-jet.

36 MATERIALS SCIENCE↗

Localizing Tungsten Single Atoms around Tungsten Nitride Nanoparticles for Efficient Oxygen Reduction Electrocatalysis in Metal–Air Batteries

Combining isolated atomic active sites with those in nanoparticles for synergizing complex multistep catalysis is being actively pursued in the design of new electrocatalyst systems. However, these novel systems have been rarely studied due to the challenges with synthesis and analysis. Herein, a synergistically catalytic performance is demonstrated with a 0.89 V (vs reversible hydrogen electrode) onset potential in the four-step oxygen reduction reaction (ORR) by localizing tungsten single atoms around tungsten nitride nanoparticles confined into nitrogen-doped carbon (W SAs/WNNC). Through density functional theory calculations, it is shown that each of the active centers in the synergistic entity feature a specific potential-determining step in their respective reaction pathway that can be merged to optimize the intermediate steps involving scaling relations on individual active centers. Impressively, the W SAs/WNNC as the air cathode in all-solid-state Zn-air and Al-air batteries demonstrate competitive durability and reversibility, despite the acknowledged low activity of W-based catalyst toward the ORR.

25 ENERGY STORAGE↗

Effect of Confinement of SIA Cluster Diffusion by Impurities on Radiation Defect Accumulation due to 14MeV neutrons in Tungsten

Impurities acting as traps, reduce the self-interstitial atom (SIA) cluster mobility, thereby increasing recombination and in turn enhancing radiation-resistance of polycrystalline materials. However, at elevated temperatures, depending on SIA-trap (impurity) binding energy, SIA clusters may trap and detrap (detach) numerous times. In tungsten, SIA clusters of all sizes glide one-dimensionally (1D) along their Burgers vector direction. Hence, detrapped SIAs would retrace their path, confining their 1D-glide between traps. However, small SIA clusters can change the direction of their 1D-glide by overcoming a rotation barrier. In addition, impurities or solutes are known to reduce this barrier. A lower rotation barrier can result in detrapped SIA clusters that diffuse in a random 1D direction, effectively leading to 3D (net-3D) diffusion. Here we investigate the effect of two cases of SIA diffusion, namely confined-1D diffusion and net-3D diffusion, on the damage accumulation in polycrystalline tungsten under 14 MeV neutron irradiation using the object kinetic Monte Carlo method. Simulations were performed using cascade debris obtained from molecular dynamics simulations with primary knock-on atom (PKA) energies corresponding to 14 MeV neutrons. In the simulations with net-3D diffusion, SIA clusters of all sizes diffuse in a random 1D direction after the clusters detrap. While for the confined 1D diffusion case, SIA clusters larger than size 5 retain their original direction of 1D-glide. In both types of simulations, trapped vacancies are assumed to be permanently immobilized. Unexpectedly, the damage accumulation was lower with confined 1D diffusion than that with net-3D. We present a systematic comparison of the influence of the two cases of SIA diffusion on the radiation damage accumulation as a function of dose rate, detrapping barrier, and impurity concentration at 1025 K.

Accumulation and recovery of lattice damage, tungs↗

Power and isotope effects in the ITER baseline scenario with tungsten and tungsten-equivalent radiators in DIII-D

Abstract Experiments in DIII-D document the ITER Baseline Scenario (IBS) at q 95 ∼ 3 and P IN / P LH ∼ 1–2, in both deuterium and hydrogen utilizing Kr and Xe as Tungsten-equivalent radiators. The power threshold for H-mode operation ( P LH ) was determined experimentally without added impurities and found to be about a factor of two higher than the scaling law. In recent IBS experiments in deuterium, intrinsic levels of metals such as Tungsten (W) or molybdenum and inconel are present that reduce the pedestal pressure by 20%–25%. A complete radiative collapse of deuterium IBS plasmas occurs at W core concentrations C W = 10 −5 . Simulations show that for core temperatures expected for ITER, the plasmas would not have a radiative collapse at C W = 1 × 10 −5 , moreover Q = 8–10 would still be achieved for C W up to 3 × 10 −5 . In contrast to deuterium, the IBS in hydrogen is not affected by intrinsic high-Z impurities, indicating that hydrogen H-modes in ITER may not inform the D-T phase with respect to W accumulation and discharge survival. Compared to deuterium, the pedestal pressure in hydrogen is ∼25% lower, with much higher ELM frequency of 150 Hz, decreasing with input power. Krypton was injected in a matrix scan of input power and impurity flow in IBS hydrogen discharges. Krypton impurity density profiles in hydrogen are similar to deuterium plasmas, but at Kr flows that are 2–3 times higher for the same input power. Krypton is transported into the core and affects the whole radius; at the highest injection rates a radiative collapse occurs at core radiation fractions of 0.3–0.35, consistent with the expected maximum W radiation fraction for ITER core plasmas. Comparing the results with previous International Tokamak Physics Activity database studies of the IBS confirms that at higher radiation fraction due to high-Z impurities, a drop in H 98 of >10% is observed. On the other hand, the results using Kr as a W-equivalent radiator indicate that metal (W) devices at lower core temperatures than ITER may provide overly pessimistic performance extrapolations to ITER for deuterium-tritium operation. The new DIII-D results support a more attractive option for the ITER Research Plan with a short hydrogen phase for system commissioning, transitioning to deuterium operations as soon as possible to provide relevant conditions for deuterium-tritium operations.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Local structure elucidation of tungsten-substituted vanadium dioxide (V$$_{1-x}$$W$$_x$$O$$_2$$)

Abstract Initially, vanadium dioxide seems to be an ideal first-order phase transition case study due to its deceptively simple structure and composition, but upon closer inspection there are nuances to the driving mechanism of the metal-insulator transition (MIT) that are still unexplained. In this study, a local structure analysis across a bulk powder tungsten-substitution series is utilized to tease out the nuances of this first-order phase transition. A comparison of the average structure to the local structure using synchrotron x-ray diffraction and total scattering pair-distribution function methods, respectively, is discussed as well as comparison to bright field transmission electron microscopy imaging through a similar temperature-series as the local structure characterization. Extended x-ray absorption fine structure fitting of thin film data across the substitution-series is also presented and compared to bulk. Machine learning technique, non-negative matrix factorization, is applied to analyze the total scattering data. The bulk MIT is probed through magnetic susceptibility as well as differential scanning calorimetry. The findings indicate the local transition temperature ( $$T_c$$ T c ) is less than the average $$T_c$$ T c supporting the Peierls-Mott MIT mechanism, and demonstrate that in bulk powder and thin-films, increasing tungsten-substitution instigates local V-oxidation through the phase pathway VO $$_2\, \rightarrow$$ 2 → V $$_6$$ 6 O $$_{13} \, \rightarrow$$ 13 → V $$_2$$ 2 O $$_5$$ 5 .

Wilson, Catrina E. (ORCID:0000000173397318)↗

Neutron irradiation-enhanced grain growth in tungsten and tungsten alloys

Herein, to understand the microstructural stability of candidate plasma-facing materials under fusion-relevant environments, neutron irradiation of W and W-3%Re alloys with and without K and La dopants was performed in the mixed-spectrum High Flux Isotope Reactor at nominal temperatures of ~850 °C and ~1100 °C to calculated doses between 0.42 and 0.47 dpa. To the best of our knowledge, this study presents the first experimental evidence of radiation-enhanced recrystallization in W and undoped W–Re alloys at ~850 °C, conditions where thermal annealing does not cause any grain growth in a similar timescale. Potassium- or lanthanum-doped tungsten alloys showed more resistance to radiation-enhanced grain growth. We explain the acceleration of grain growth by analyzing the self-diffusion constant under atomic displacement environments. The microstructural observations of the studied W variants suggest that La doping is more effective than K doping for mitigating recrystallization. This study also found that radiation-enhanced recrystallization is an important consideration when designing and applying W to plasma-facing components in future nuclear fusion reactors.

36 MATERIALS SCIENCE↗

Origins of wear-induced tungsten corrosion defects in semiconductor manufacturing during tungsten chemical mechanical polishing

During chemical mechanical polishing (CMP) process optimization, a unique corrosion defect was identified in the tungsten (W) contact plugs, which were investigated to develop practical solutions to improve CMP mass productivity. The corrosion defect occurred in the absence of external incident energy and was observed to occur only at the W plugs connected to the P + /n-well close to the wafer edge. To examine the root cause of the corrosion, a series of experiments was carried out at each W CMP step, using in-line defect inspection. Additional experiments were conducted using on-line inductively coupled plasma mass spectrometry (ICP-MS) to understand pH- and potential-dependent electrochemical dissolution behaviors of W. Experimentally, W corrosion was confirmed to be exacerbated if the surface oxide of the W plugs is removed by the deionized water (DIW) rinsing step under wafer pressurization, then exposed to DIW and alkaline cleaning solution. Although the DIW rinsing step is commonly performed to clean polishing pads right after the main polishing, a small amount of applied pressure (0.5 psi) without slurry supply can lead to corrosion defects. Finally, this wear-induced corrosion of the W plugs can be prevented by removing the applied pressure during the post DIW rinsing step of W CMP.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Stability and mobility of tungsten clusters on tungsten (110) surface: Ab initio and atomistic simulations

Quantifying the surface transport properties of tungsten (W) is of prime importance to understand the formation of nano-fuzz in fusion plasma-facing conditions. The stability and mobility of W adatom clusters (W n , n = 2-9) on the W(110) surface has been investigated by computer simulations, including ab initio calculations using density functional theory (DFT) and molecular statics (MS) simulations with multiple W interatomic potentials. The DFT results demonstrate that the sequential binding energy generally increases with number of W adatoms, except for the 5 th and 7 th W adatoms. The most common elemental migration steps of W n (n>2) clusters are observed to consist of monomer and dimer hops, while larger W n clusters can also diffuse by dissociation and recombination of smaller clusters. The threshold migration energy of W 9 is the highest, then followed by W 8 , W 4 , and W 6 , while W 3 , W 5 , and W 7 have similar migration energies. Compared to DFT, each interatomic potential evaluated overestimates the binding energies of W n clusters. Additionally, the embedded-atom potential developed by Juslin and Wirth adequately predicts the threshold migration energy of W n (n>2) clusters, although it predicts different underlying migration mechanisms. The results show that interaction mechanism between W adatoms controls the stability and mobility of W n clusters on the W(110) surface.

36 MATERIALS SCIENCE↗