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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 379 records · Page 21
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

In Situ Neutron Scattering Study of the Structure Dynamics of the Ru/Ca 2 N:e – Catalyst in Ammonia Synthesis

NH 3 synthesis is one of the most critical industrial processes. Compared to commercial iron catalysts, Ru catalysts show high intrinsic activity in this reaction but suffer from hydrogen poisoning. By loading Ru onto supports such as electrides and hydrides, the hydrogen poisoning problem can be significantly alleviated. However, relevant studies on the structural dynamics of the Ru/electride catalysts under reaction conditions are very scarce. Taking advantage of the high sensitivity to hydrogen species, it is possible to obtain insights into the structural changes during the reaction using in situ neutron techniques. In this study, we have investigated the structural evolution of the Ru/Ca 2 N:e – catalyst during the ammonia synthesis reaction by in situ neutron scattering (inelastic neutron scattering, INS) technique. In situ INS experiments suggest that Ca 2 N:e – is likely converted to the Ca 2 NH phase during the reaction. Unlike the previously known structure where H and N atoms are intermixed, the formed Ca 2 NH exhibits a segregated structure where the H and N atoms are located in different layers separated by the Ca layer. In conclusion, density functional theory calculations of the reaction energetics reveal that there are minor changes in the barriers and thermodynamics of the first N hydrogenation step between the two phases (Ca 2 NH phase with segregated H/N layers and intermixed Ca 2 NH phase), suggesting the impact of the phases on the reaction kinetics to be relatively minimal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Reformulated Red mud: a robust catalyst for in situ catalytic pyrolysis of biomass

Biomass feedstocks contain inorganic compounds generally classified as ash. The ash consists of compounds of potassium, calcium, magnesium, silicon, phosphorous and other elements. These elements have been reported to influence both the pyrolysis reactions as well as destabilizing the pyrolysis oils during storage. The inorganic elements have also been reported to deposit on catalyst surfaces during in situ catalytic pyrolysis leading to the eventual deactivation of acidic catalysts such as zeolites. The deposition of inorganic elements and their effect on formulated red mud (FRM) catalyst during in situ catalytic pyrolysis of pinyon juniper wood was investigated. The inorganic elements were measured for the fresh, coked, and regenerated catalysts. The BET specific surface area of the FRM catalyst decreased from 76 m2/g for the fresh catalyst to 53 m2/g for the stable regenerated catalyst. After three regenerations, the BET specific surface area stabilized at 53 m2/g and remained constant after all other regenerations. Potassium, calcium, magnesium, and phosphorous were deposited on the catalyst. Potassium deposition was linear with the number of regenerations while magnesium and calcium depositions were initially rapid but leveled off after three regenerations of the catalyst. Phosphorous deposition was almost linear, but the data were more scattered compared to potassium. The potassium deposition was attributed to physical phenomenon whereas calcium and magnesium depositions were more akin to chemical reactions related to the loss of BET surface area of the catalyst. The deposition of these elements on the surface of the catalyst did not deactivate it. After each catalyst regeneration, the oil yield was not significantly affected and the oil oxygen content and viscosity decreased slightly. This clearly showed that formulated red mud is a robust catalyst suitable for in situ catalytic fast pyrolysis of biomass.

Agblevor, Foster↗
DOE OSTI2020

Relationship among the Crystal Structure, Texture, and Macroscopic Properties of Tetragonal (Pb,La)(Zr,Ti)O 3 Ferroelectrics Investigated by In Situ High-Energy Synchrotron Diffraction

In situ diffraction investigations have played an important role in experimentally revealing the mechanism of piezoelectric and ferroelectric properties. In this study, a pure tetragonal ferroelectric ceramic of La-doped PbZr 0.5 Ti 0.5 O 3 (LaPZT50) was investigated to eliminate the complex influence of phase coexistence. The electric field evolutions of the crystal structure, domain switching, and lattice deformation of the tetragonal phase have been revealed by in situ high-energy synchrotron X-ray diffraction. Furthermore, we found that the crystal structure of LaPZT50 is quite stable, showing a negligible change in the Pb–O bond length, unit cell volume, and spontaneous polarization upon application of an in situ external electric field. Importantly, the maximum macroscopic polarization of tetragonal LaPZT50 is defined by the 111-oriented grains. As determined by the intensity difference, the switching of non-180° domains plays a more significant role in contributing to the macroscopic strain than lattice deformation. These results further imply that the phase coexistence around the morphotropic phase boundary facilitates domain wall motion in the tetragonal phase and improves the ferroelectric and piezoelectric properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Electrolyte/Dye/TiO 2 Interfacial Structures of Dye-Sensitized Solar Cells Revealed by In Situ Neutron Reflectometry with Contrast Matching

The nature of an interfacial structure buried within a device assembly is often critical to its function. For example, the dye/TiO 2 interfacial structure that comprises the working electrode of a dye-sensitized solar cell (DSC) governs its photovoltaic output. These structures have been determined outside of the DSC device, using ex situ characterization methods; yet, they really should be probed while held within a DSC since they are modulated by the device environment. Dye/TiO 2 structures will be particularly influenced by a layer of electrolyte ions that lies above the dye self-assembly. We show that electrolyte/dye/TiO 2 interfacial structures can be resolved using in situ neutron reflectometry with contrast matching. Here, we find that electrolyte constituents ingress into the self-assembled monolayer of dye molecules that anchor onto TiO 2 . Some dye/TiO 2 anchoring configurations are modulated by the formation of electrolyte/dye intermolecular interactions. These electrolyte-influencing structural changes will affect dye-regeneration and electron-injection DSC operational processes. This underpins the importance of this in situ structural determination of electrolyte/dye/TiO 2 interfaces within representative DSC device environments.

14 SOLAR ENERGY↗
DOE OSTI2022

Dynamics of Polymer Nanocapsule Buckling and Collapse Revealed by In Situ Liquid-Phase TEM

Nanocapsules are hollow nanoscale shells that have applications in drug delivery, batteries, self-healing materials, and as model systems for naturally occurring shell geometries. In many applications, nanocapsules are designed to release their cargo as they buckle and collapse, but the details of this transient buckling process have not been directly observed. In this work, we use in situ liquid-phase transmission electron microscopy to record the electron-irradiation-induced buckling in spherical 60-187 nm polymer capsules with ~3.5 nm walls. We observe in real time the release of aqueous cargo from these nanocapsules and their buckling into morphologies with single or multiple indentations. The in situ buckling of nanoscale capsules is compared to ex situ measurements of collapsed and micrometer-sized capsules and to Monte Carlo (MC) simulations. The shape and dynamics of the collapsing nanocapsules are consistent with MC simulations, which reveal that the excessive wrinkling of nanocapsules with ultrathin walls results from their large Föppl-von Kármán numbers around 10 5 . Our experiments suggest design rules for nanocapsules with the desired buckling response based on parameters such as capsule radius, wall thickness, and collapse rate.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Discriminating the Role of Surface Hydride and Hydroxyl for Acetylene Semihydrogenation over Ceria through In Situ Neutron and Infrared Spectroscopy

Ceria has been used as a hydrogenation catalyst especially in selective alkyne hydrogenation, but the reaction mechanism regarding the role of different surface hydrogen species remains unclear. Here, we utilized in situ neutron and infrared vibration spectroscopy to show the catalytic role of cerium hydride (Ce–H) and hydroxyl (OH) groups in acetylene hydrogenation over ceria surfaces with different degree of reduction. In situ inelastic neutron scattering spectroscopy (INS) proved that not only Ce–H but also surface atomic hydrogen species on the reduced ceria surface can participate in acetylene semihydrogenation. In situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) results implied that bridging OH groups both on the oxidized and reduced ceria are active in the selective hydrogenation of acetylene. It appears that surface Ce–H is more reactive than the coexisting OH species on the reduced ceria surface, but over-reduction of ceria also results in strongly bound species that may lead to catalyst deactivation. These spectroscopic results clearly explain the reaction mechanism including not only the surface chemistry but also the nature of the active hydrogen species for selective hydrogenation over ceria, providing insights into the design of more active and stable ceria-based catalysts for hydrogenation reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

In Situ Strong Metal–Support Interaction (SMSI) Affects Catalytic Alcohol Conversion

Strong metal–support interactions (SMSIs) and catalyst deactivation have been heavily researched for decades by the catalysis community. The promotion of SMSIs in supported metal oxides is commonly associated with H 2 treatment at high temperature (>500 °C), and catalyst deactivation is commonly attributed to sintering, leaching of the active metal, and overoxidation of the metal, as well as strong adsorption of reaction intermediates. Alcohols can reduce metal oxides, and thus here we have hypothesized that catalytic conversion of alcohols can promote SMSIs in situ . In this work we show, via IR spectroscopy of CO adsorption and electron energy loss spectroscopy (EELS), that during 2-propanol conversion over Pd/TiO 2 coverage of Pd sites occurs due to SMSIs at low reaction temperatures (as low as ~ 190 °C). The emergence of SMSIs during the reaction ( in situ ) explains the apparent catalyst deactivation when the reaction temperature is varied. A steady-state isotopic transient kinetic analysis (SSITKA) shows that the intrinsic reactivity of the catalytic sites does not change with temperature when SMSI is promoted in situ ; rather, the number of available active sites changes (when a TiO x layer migrates over Pd NPs). SMSI generated during the reaction fully reverses upon exposure to O 2 at room temperature for ~15 h, which may have made their identification elusive up to now.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

In Situ EXAFS Study of Mo–P Bond Dynamics in Molybdenum Phosphide during CO 2 Reduction and Hydrogen Evolution

Transition Metal Phosphides (TMPs) are widely studied as catalysts in reactions like hydrogen evolution, oxygen reduction, and hydrodesulfurization. TMPs have demonstrated remarkable efficiency in accelerating reactions by providing active sites for adsorption and facilitating the transformation of reaction intermediates, a feature that has increased the interest of TMPs in the electrochemical carbon dioxide reduction reaction (eCO 2 RR). Despite their growing use, the potential-dependent structural behavior of TMPs under operating electrochemical conditions remains insufficiently understood. This work investigates the dynamics of the Mo−P bond during eCO 2 RR and hydrogen evolution reaction (HER) using in situ extended X-ray absorption spectroscopy (EXAFS) studies at the Mo−K edge. Structural characterization of the synthesized MoP nanoparticles was performed by powder X-ray diffraction (XRD) and transmission electron microscopy (TEM). Results of the overall electrochemical activity of MoP are presented through linear sweep voltammetry (LSV) experiments in the potential range of 0 to −1.5 V versus Ag/AgCl and chronoamperometry (CA). Liquid products were analyzed by 1 H NMR spectroscopy. The synthesized catalyst showed increasing activity with the highest Faradaic efficiency of 11.75% for C 2+ products at −1.3 V vs Ag/AgCl. In situ EXAFS revealed a change in the average Mo−P bond distance during eCO 2 RR, whereas no such change was observed during the hydrogen evolution reaction (HER). This finding suggests that phosphorus, particularly through modulation of the Mo−P bond length, plays an important role in the eCO 2 RR and demonstrates how in situ EXAFS can track local structural perturbations in MoP catalysts during electrochemical operation, providing complementary structural insight that correlates with electrochemical behavior.

Catalysts↗
DOE OSTI2020

Oxidation State and Surface Reconstruction of Cu under CO 2 Reduction Conditions from In Situ X-ray Characterization

The electrochemical CO 2 reduction reaction (CO 2 RR) using Cu-based catalysts holds great potential for producing valuable multi-carbon products from renewable energy. However, the chemical and structural state of Cu catalyst surfaces during the CO 2 RR remains a matter of debate. In this paper, we show the structural evolution of the near-surface region of polycrystalline Cu electrodes under in situ conditions through a combination of grazing incidence X-ray absorption spectroscopy (GIXAS) and X-ray diffraction (GIXRD). The in situ GIXAS reveals that the surface oxide layer is fully reduced to metallic Cu before the onset potential for CO 2 RR, and the catalyst maintains the metallic state across the potentials relevant to the CO 2 RR. We also find a preferential surface reconstruction of the polycrystalline Cu surface toward (100) facets in the presence of CO 2 . Quantitative analysis of the reconstruction profiles reveals that the degree of reconstruction increases with increasingly negative applied potentials, and it persists when the applied potential returns to more positive values. These findings show that the surface of Cu electrocatalysts is dynamic during the CO 2 RR, and emphasize the importance of in situ characterization to understand the surface structure and its role in electrocatalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

In Situ Imaging of Faujasite Surface Growth Reveals Unique Pathways of Zeolite Crystallization

Zeolite crystallization occurs by complex processes involving a variety of possible mechanisms. The sol gel media used to prepare zeolites leads to heterogeneous mixtures of solution and solid states with diverse solute species. At later stages of zeolite synthesis when growth occurs predominantly from solution, classical two-dimensional nucleation and spreading of layers on crystal surfaces via the addition of soluble species is the dominant pathway. At earlier stages, these processes occur in parallel with nonclassical pathways involving crystallization by particle attachment (CPA). The relative roles of solution- and solid-state species in zeolite crystallization have been a subject of debate. Here, in this work, we investigate the growth mechanism of a commercially relevant zeolite, faujasite (FAU). In situ atomic force microscopy (AFM) measurements reveal that supernatant solutions extracted from a conventional FAU synthesis at various times do not result in growth, indicating that FAU growth predominantly occurs from the solid state through a disorder-to-order transition of amorphous precursors. Elemental analysis shows that supernatant solutions are significantly more siliceous than both the original growth mixture and the FAU zeolite product; however, in situ AFM studies using a dilute clear solution with a lower Si/Al ratio revealed three-dimensional growth of surfaces that is distinct from layer-by-layer and CPA pathways. This unique mechanism of growth differs from those observed in studies of other zeolites. Given that relatively few zeolite frameworks have been the subject of mechanistic investigation by in situ techniques, these observations of FAU crystallization raise the question whether its growth pathway is characteristic of other zeolite structures.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Constraining Erosion Rates and Landscape Evolution With In Situ 10 Be and 26 Al Cosmogenic Nuclides at Table Mountain, Antarctica

Abstract This study investigates surface weathering and sediment preservation at Table Mountain, a high‐elevation, hyperarid, polar landscape in the Transantarctic Mountains. We report cosmogenic nuclide concentrations ( 10 Be and 26 Al) in quartz from bedrock surfaces, erratic boulder lag, and cobbles embedded within Sirius Group sediments to quantify erosion rates. In situ 10 Be and 26 Al depth profiles from a 2.95 m permafrost core in the Sirius Group further constrain surface erosion rates and elucidate landscape stability. Measured 10 Be and 26 Al concentrations from two sandstone bedrock surfaces adjacent to Sirius Group sediments give erosion rates of 0.18–0.28 m/Myr. An erratic sandstone boulder within the lag above the Sirius Group yields erosion rates of ∼0.42 ± 0.03 m/Myr, whereas two cobbles embedded within the Sirius Group yield higher rates of 0.81–1.12 m/Myr. Depth profiles of in situ 10 Be and 26 Al indicate no vertical mixing of Sirius Group permafrost since deposition. Depth profile models are best explained by erosion rates of 0.53 +0.13 / −0.12 m/Myr, and an exposure age of 0.78 +0.06 / −0.08 Ma. We view the model “age” to represent the ∼0.8‐million‐year time‐scale for surface lowering equivalent to one attenuation length of cosmic ray production to achieve steady‐state conditions. Continual exhumation of embedded clasts from within the Sirius Group results in an accumulation of clasts forming the observed erosional lag deposit covering the landscape. Our erosion rates of the Sirius Group surface based on in situ 10 Be and 26 Al depth profiles are an order‐of‐magnitude larger than those based on meteoric 10 Be infiltration and further clarification is required.

58 GEOSCIENCES↗
DOE OSTI2025

Best practices for in-situ and operando techniques within electrocatalytic systems

In-situ and operando techniques in heterogeneous electrocatalysis are a powerful tool used to elucidate reaction mechanisms. Ultimately, they are key in determining concrete links between a catalyst’s physical/electronic structure and its activity en route to designing next-generation systems. To this end, the exact execution and interpretation of these lines of experiments is critical as this determines the strength of conclusions that can be drawn and what uncertainties remain. Instead of focusing on how techniques were used to understand systems, as is the case with most reviews on the topic, this work instead initiates a nuanced discussion of 1) how to best carry out each technique and 2) initiate a nuanced analysis of which level of insights can be drawn from the set of in-situ or operando experiments/controls carried out. We focus on several commonly used techniques, including vibrational (IR, Raman) spectroscopy, X-ray absorption spectroscopy and electrochemical mass spectrometry. In addition to this, we include sections of reactor design and the link with theoretical modelling that are applicable across all techniques. While we focus on heterogeneous electrocatalysis, we make links when appropriate to the areas of photo- and thermo-catalytic systems. We highlight common pitfalls in the field, how to avoid them, and what sets of complementary experiments may be used to strengthen the analysis. We end with an overview of what gaps remain in in-situ and operando techniques and what innovations must be made to overcome them.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Low-temperature and effective ex situ group V doping for efficient polycrystalline CdSeTe solar cells

CdTe solar cell technology is one of the lowest-cost methods of generating electricity in the solar industry, benefiting from fast CdTe absorber deposition, CdCl 2 treatment and Cu doping. However, Cu doping has low photovoltage and issues with instability. Doping group V elements into CdTe is therefore a promising route to address these challenges. Although high-temperature in situ group V doped CdSeTe devices have demonstrated efficiencies exceeding 20%, they face obstacles including post-deposition doping activation processes, short carrier lifetimes and low activation ratios. Here, we demonstrate low-temperature and effective ex situ group V doping for CdSeTe solar cells using group V chlorides. For AsCl 3 doped CdSeTe solar cells, the dopant activation ratio can be 5.88%, hole densities reach >2 × 10 15 cm -3 and carrier lifetime is longer than 20 ns. Thus, ex situ As doped CdSeTe solar cells show open-circuit voltages ~863 mV, compared to the highest open-circuit voltage of 852 mV for Cu doped CdSeTe solar cells.

14 SOLAR ENERGY↗
DOE OSTI2021

Predicting Thermal Excursions During in situ Oxidative Regeneration of Packed Bed Catalytic Fast Pyrolysis Catalyst

Ex situ catalytic fast pyrolysis (CFP) uses a secondary reactor to upgrade biomass pyrolysis vapors to stabilized CFP oils with reduced oxygen content. In one configuration, the secondary reactor is operated as a packed-bed swing reactor system which allows coke-deactivated beds to be decarbonized in situ while other beds remain online for vapor upgrading. In situ decarbonization must be done carefully to avoid irreversible deactivation and/or physical degradation of catalyst pellets. Given that packed bed reactors are well known to have poor heat transfer characteristics, this is a critical issue impacting scaleability and commercial viability of the technology. To predict thermal excursions during regeneration, finite element computational models have been built to assist in scaling up oxidative decarbonization of a Pt/TiO2 CFP catalyst (0.5 mm spheres) from a bench scale packed bed with 100 g of catalyst to a pilot scale packed bed with 2 kg of catalyst and internal cooling tubes. Based on transient measurements of outlet temperature and effluent CO2 concentration, and using an assumed coke profile and activation energy, this paper demonstrates that specific combinations of effective thermal conductivity and wall heat transfer coefficient can fit bench scale oxidative regeneration data equally well. For the upscaled 2 kg bed, four bench-scale “best fit” parameter pairs give different predictions for location and magnitude of thermal excursions, with the maximum computed bed temperature gradients ranging from 30 °C cm-1 to as high as 3000 °C cm-1. The larger the fraction of heat removal by conduction through the cooling tubes, the greater the differences between the parameter pairs. The modelling results presented in this paper cast doubt on the industrial viability of the proposed combination of catalyst, bed and regeneration process, and point to the need for alternate reactor designs. However, there is considerable uncertainly in some of the key model parameters. The reliability of model predictions can be increased by adding more temperature measurements at key bed locations, testing additional variations in process conditions, performing careful bed dissections to determine the true coke profile, and perhaps most importantly, directly measuring the effective thermal conductivity of the catalyst pellets.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Wisconsin In Situ Penning (WISP) gauge: A versatile neutral pressure gauge to measure partial pressures in strong magnetic fields

A new type of in-vessel Penning gauge, the Wisconsin In Situ Penning (WISP) gauge, has been developed and successfully operated in the Wendelstein 7-X (W7-X) island divertor baffle and vacuum vessel. The capacity of the quantitative measurements of the neutral reservoir for light impurities, in particular, helium, is important for tokamaks as well as stellarator divertors in order to avoid fuel dilution and radiative energy loss. Penning gauges assisted by spectroscopy are a powerful tool to obtain the total neutral pressure as well as fractional neutral pressures of specific impurities. The WISP gauge is a miniaturized Penning gauge arrangement, which exploits the ambient magnetic field of magnetic confinement fusion experiments to establish the Penning discharge. Then, in situ spectroscopy is conducted to separate the fractional neutral pressures of hydrogen, helium, and possibly also other impurities. The WISP probe head was qualified using the magnetic field of the Magnetized Dusty Plasma Experiment at Auburn University between 0.25 T and 3.5 T [E. Thomas et al ., J. Plasma Phys. 81, 345810206 (2015)]. The in-depth quantitative evaluation for hydrogen and helium will be shown as well as an exploration of nitrogen, argon, and neon. A power law scaling between current I and pressure p, I = f (Gas,V) p n⁽Gas, B⁾ , was shown. The factor f is gas and anode potential dependent, while n is gas and magnetic field strength dependent. Pressure measurements from 0.1 mbar and down to 1 × 10 -5 mbar were achieved, demonstrating a reliable operating range for relevant pressure levels in the divertor and main vessel regions in current and future fusion devices, with a time resolution of up to 1 kHz. The lowest achievable pressure measurement increases with an increase in B and can be shifted with the anode potential V . At W7-X, the WISP probe head was mounted on an immersion tube setup that passes through the cryostat and places the probe head close to the plasma. Two probe heads were positioned in different divertor pump gaps, top and bottom, and one close to the plasma on the midplane in one module. The gauges were in situ calibrated together with the ASDEX pressure gauges [G. Haas and H.-S. Bosch, Vacuum 51, 39 (1998)]. Data were taken during the entire operation phase 1.2b, and measurements were coherent with other neutral gas pressure gauges. For the spectroscopic partial pressure measurements, channels of a spectroscopic detection system based on photo-multipliers, a so-called filterscope [R. J. Colchin et al ., Rev. Sci. Instrum. 74, 2068 (2003)], provided by the Oak Ridge National Lab were used.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

In situ x-ray and electron scattering studies of oxide molecular beam epitaxial growth

We perform the first in situ synchrotron X-ray ray diffraction (SXRD) / reflection high energy electron diffraction (RHEED) studies on the growth of complex oxide thin films by molecular beam epitaxy. The unique deposition chamber, located at the Advanced Photon Source, allows the preparation of complex oxide samples with monolayer precision and facilitates the formation of direct correlations between in situ X-ray studies and the more prevalent RHEED investigations. Importantly, because SXRD and RHEED probe different atomic-scale processes during thin film synthesis, their concomitant use enables the extraction of details concerning growth behavior than one cannot determine from either probe alone. We describe the results of such in situ studies on the epitaxial growth of perovskite LaNiO3on (La 0.18 Sr 0.82 )(Al 0.59 Ta 0.41 )O 3 (001). We find that during the earliest stages of growth, the RHEED and X-ray signals do not agree with each other, demonstrating that while regular RHEED oscillations may imply high quality growth, the film-substrate interface can undergo significant changes during deposition due to the occurrence of interdiffusion at the growth temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2021

A digital holography ex situ measurement characterization of plasma-exposed surface erosion from an electrothermal arc source

Digital holography has been proposed to fulfill a need for an imaging diagnostic capable of in situ monitoring of surface erosion caused by plasma–material interaction in nuclear fusion devices. A digital holography diagnostic for 3D surface erosion measurement has been developed at Oak Ridge National Laboratory with the goal of deployment on a plasma device. A proof-of-concept in situ demonstration is planned which would involve measurement of plasma erosion on targets exposed to an electrothermal arc source. This work presents the results of an ex situ characterization of the capability and limitations of holographic imaging of targets exposed to the arc source. Targets were designed to provide a fiducial for comparison of deformed and unaffected areas. The results indicated that the average net erosion was ~150 nm/plasma exposure, which is expected to be within the diagnostic’s measurement capacity. Surface roughness averages determined by holographic image analysis showed good agreement with measurements taken with a profilometer. Finally, the limit of the holography diagnostic’s x–y spatial resolution was characterized by comparison with scanning electron microscope imaging.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

In-situ coating of silicon-rich films on tokamak plasma-facing components with real-time Si material injection

Abstract Experiments have been conducted in the DIII-D tokamak to explore the in-situ growth of silicon-rich layers as a potential technique for real-time replenishment of surface coatings on plasma-facing components (PFCs) during steady-state long-pulse reactor operation. Silicon (Si) pellets of 1 mm diameter were injected into low- and high-confinement (L-mode and H-mode) plasma discharges with densities ranging from 3.9– 7.5 × 10 19 m −3 and input powers ranging from 5.5 to 9 MW. The small Si pellets were delivered with the impurity granule injector at frequencies ranging from 4 to 16 Hz corresponding to mass flow rates of 5–19 mg s −1 (1– 4.2 × 10 20 Si s −1 ) at cumulative amounts of up to 34 mg of Si per five-second discharge. Graphite samples were exposed to the scrape-off layer and private flux region plasmas through the divertor material evaluation system to evaluate the Si deposition on the divertor targets. The Si II emission at the sample correlates with silicon injection and suggests net surface Si-deposition in measurable amounts. Post-mortem analysis showed Si-rich coatings containing silicon oxides, of which SiO 2 is the dominant component. No evidence of SiC was found, which is attributed to low divertor surface temperatures. The in-situ and ex-situ analysis found that Si-rich coatings of at least 0.4–1.2 nm thickness have been deposited at 0.4–0.7 nm s −1 . The technique is estimated to coat a surface area of at least 0.94 m 2 on the outer divertor. These results demonstrate the potential of using real-time material injection to form Si-enriched layers on divertor PFCs during reactor operation.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗