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DOE OSTI2021

Multiscale Catalytic Fast Pyrolysis of Grindelia Reveals Opportunities for Generating Low Oxygen Content Bio-Oils from Drought Tolerant Biomass

Grindelia squarrosa (curlycup gumweed) biomass possesses unique biochemistry, cell wall composition, and leaf architecture tailored for prolific growth in arid and semiarid climates. Most notably, this plant has developed high levels of extractable resins that have high effective H/C eff ratios ((mol H - 2 x mol O)/mol C), which is hypothesized to lead to low coke formation during catalytic fast pyrolysis (CFP) over the ZSM-5 catalyst. In microscale experiments with high ZSM-5 loadings (biomass-to-catalyst mass ratio (B/C) ~ 0.1), in situ CFP generated high yields of aromatic hydrocarbons (30% carbon yield) while ex situ CFP favored aliphatic hydrocarbons (25% carbon yield). The difference between the two configurations was attributed to the constant catalyst temperature during ex situ CFP. Deactivation leading to partially deoxygenated vapor products occurred rapidly until B/C ≤ 0.5 by the adsorption of organic species blocking access to acid sites inside the micropores of the catalyst. This was followed by more gradual deactivation leading to primary vapor breakthrough, which we attribute to coke formation on acid sites on the external surface of ZSM-5 crystallites. Noncatalytic fast pyrolysis of Grindelia in a bench scale reactor produced oils with oxygen content (18 wt % on dry basis) and carbon yield (33%) comparable to those of CFP of woody biomass. The CFP of Grindelia further reduced the oxygen content to 7 wt % for in situ CFP and 4 wt % for ex situ CFP at B/C of 2-3. The good deoxygenation was attributed to a combination of a high H/C eff ratio and overall better quality of the pyrolysis vapors that were passed over the ZSM-5 catalyst. The high inorganic content of the Grindelia likely catalyzed pyrolysis to remove oxygenated coke precursors. This integrated CFP study demonstrated that Grindelia could be an important feedstock for generating stabilized noncatalytic and CFP oils for downstream processing into fuels and/or extraction of high-value chemicals. The preprocessing of this feedstock will be required to remove inorganics, which cause an irreversible deactivation of ZSM-5.

BIOMASS FUELS↗

DOE OSTI2023

Conference Report on the 7th International Symposium on Liquid metals Applications for fusion (ISLA-7)

Supported by the world magnetic fusion research community, a series of International Symposia on Liquid metals Applications for fusion (ISLA) have been held biannually since 2010. The 7th edition (ISLA-7) was held for the period from 12 December through 16 December 2022, at Chubu University located in Kasugai, Aichi, Japan. For the first time in the history of this series of symposia, ISLA-7 was held in a hybrid fashion, due to the COVID-19 situation. The total number of the participants was 60, 34 out of whom attended the symposium in person, and the rest participated online. As to the presentation statistics, 29 papers were presented in person, whereas 21 presentations were delivered online but real-time by the presenters in China, Spain, the UK, and the USA. Both of the presentations delivered in person and online were recorded, and the video has been shared by all participants. These participants represent 11 countries: China, Czech, Italy, Japan, Latvia, Netherlands, Russia, Thailand, the UK, and the USA. All these numbers are among the largest in this series of symposia. Covered by these presentations are; in session-2, program overviews and liquid metal research review; in session-3, liquid metal flows, and MHD issues; in session-4, liquid metal facilities; in sessions-5 and 6, liquid metal experiments and modeling; in session-7, divertor physics and heat flux mitigation; in session-8, plasma and liquid metals interactions; in session-9 liquid metal plasma-facing components, erosion, and wettability. In addition, there were an opening session whereby several opening addresses were delivered and also a closing session where all technical session summaries were presented by the respective session chairs.

divertor↗

DOE OSTI2023

Multi-Sourced Collaboration for the Production and Refining of Rare Elements and Critical Metals (Final Technical Report)

The project objective was to develop a feasible and cost-effective method for recovering rare earth elements (REEs) and critical materials (CMs) from coal and coal byproducts, resulting in high-purity individually separated REEs and CMs. The targeted REEs included Y, Pr, Nd, Gd, Dy, and Sm, with a purity of over 99.5%, while the CMs included Co, Mn, Ga, Sr, Li, Ni, Zn, and Ge, with a purity of over 90%. The project aimed to design a prototype facility capable of producing 1-3 tonnes/day of high-purity REO mixes. The work was divided into four designated circuits: 1) REE extraction and concentration, 2) REE separation and purification, 3) RE metal production, and 4) CM production. To achieve these goals, the project involved 11 tasks, including technology reviews, research, process flow diagram development, mass balance estimation, and preliminary technical-economic analysis. The project team included researchers from the University of Kentucky, University of Alabama and Virginia Tech as well as process specialists from Argonne National Laboratory. MP Materials provided technical support regarding rare earth markets and processing while Alliance Coal performed resource assessment. The project included a market analysis for Nd/Pr, Tb, Dy, Gd, Y, Co, Mn, Li, Sr, Ga, Ni, Zn, and Ge. These analyses provided insights into the supply and demand trends as well as historic and future projections of market price relative to purity requirements for these elements. Two coal resources were selected for the project: the West Kentucky No. 13 (Baker) Seam and an undisclosed lignite resource in the Illinois coal basin. The estimated quantities of REEs in these resources were calculated based on production samples and drilling data. It was estimated that there is adequate supply for an operation producing one metric ton daily of higher purity mixed rare earth oxides (MREO) for approximately 20 years at a site located in western Kentucky. In Circuit 1, project data was obtained from a pilot heap leach and REE concentration facility. It was concluded that the existing circuit, which generated a MREO concentrate, two types of CM mixed products, and Li- and Sr-containing waters, would be suitable feed for circuits 2-4. Data from the first-of-its-kind coal coarse refuse heap leach pilot pad played a crucial role in estimating reliable elemental concentrations of the pregnant leaching solution (PLS). The average total REE concentration in the PLS was found to be 28.6 ppm. In Circuit 2, several concepts were explored including a novel process referred to as solvent-assisted chromatography (SAC). This concept involved a novel columnar reactor that incorporated multiple mixer/settlers, thereby enabling the operation of counter-flowing aqueous and organic phases. Unfortunately, due to project time constraints, a complete fundamental modeling analysis could not be completed to fully evaluate the technology. Molten salt electrowinning was considered as an alternative for circuit 3 following circuit 2 purification circuit utilizing the novel SAC process. A mass and energy balance of Nd reduction to metal in a fluoride containing molten salt electrolyte was conducted. Comparisons were made with the current state of Asian molten salt electrorefining, and potential improvements in siphoning rare earth metals (REM) from the reactor were presented. A cost estimate was performed for the production of 1 tonne per day, which yielded a total of $2.29 million for the nine electrowinning (EW) cells required. The selected option for circuits 2 and 3 was a plasma distillation process, which initially separates rare earth elements (REEs) from other elements. This is followed by selective electrowinning in various ionic liquids. The selection was made on the basis of thermodynamic modeling and experimental data previously published by a project partner. The combination offers an innovative approach to integrated refining and RE metal production. For Circuit 4, an extensive literature review was conducted for the processing of the CMs. The ultimate decision was to utilize a combined plasma and ionic liquid process as well to produce individual high-purity concentrates of Zn, Ni, Co, Mn, and Mg. A separate flowsheet for Li and Sr was recommended, which would yield carbonates of these elements. Due to the lack of suitable experimental data at this time, a process recommendation could not be provided but several methods have been proposed for consideration. Lastly, a techno-economic analysis (TEA) was conducted to assess the effectiveness of the proposed process for further investigation. The TEA results revealed a capital expense (CapEx) of $737 million and an annual operational expense (OpEx) of $220 million. Due to the selected elements, the hypothetical heap leach pad can produce 1 metric tonne per day of REO equivalent, but a conscious decision was made to only treat targeted REEs, resulting in the production of 0.4 metric tonne of REM. An estimated annual revenue of $90.87 million was projected based on standard market pricing information provided by the funding agency. During the TEA, ten different modules were evaluated for costing purposes. The precipitation circuit was identified as the largest single operational expense, followed by the Mg/Mn process due to the amount of treated metal. In terms of capital expenditures, the heap leach process incurred the highest cost, followed by the Mg/Mn process. The scalability of the plasma process is a crucial consideration since the reactors cannot be scaled beyond the largest demonstrated size due to their reliance on surface area of the slag and vapor phase. The purity estimate for the REEs are generally 98%±2% to produce a metal. The purity level being lower than the project objective was due to the lack of specific experimental data needed to tighten the tolerance of the estimates. Based on literature and previous experience, the CMs are estimated as follows; Ga (95%+, metal), Sr (95%+, carbonate), Li (95%+, carbonate), Ni (98%±2%, metal), Zn (95%+, metal sponge), Ge (95%+, metal), Co (98%±2%, metal), and Mn (98%±2%, metal).

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2025

Assessment of Benefits of Solid-State Advanced Manufacturing Processes for Nuclear Energy Products

The Advanced Materials and Manufacturing Technology (AMMT) program develops cross cutting technologies in support of a broad range of nuclear reactor technologies and maintains U.S. leadership in materials and manufacturing technologies for nuclear energy applications. This overall project provides the U.S. Department of Energy a critical feasibility study comparison of three solid-state processes to other AM processes, thereby providing the feasibility of the solid-state processes examined to manufacture 316H SS and ODS steel components: • Fused-filament fabrication (FFF): This work provides an initial evaluation of the impact of powder morphology and sizes on the FFF process, and the feasibility and adaptability for different material systems, to use FFF for ODS steels and 316 SS. • Shear-assisted processing and extrusion (ShAPE): Specifically for this portion of the project on ShAPE tube forming, the objectives will be to determine the feasibility to direct tube forming of high tensile strength steel tubing, specifically for ODS steel to determine the effect of the patented extrusion process on the dispersoids of the ODS material. Additionally, as often ODS powders are mechanically alloyed and therefore more platelike or angular, this feasibility was to explore the impact on the optimization process and initial feasibility of direct tube forming. • Cold spray and friction stir additive manufacturing as a stretch goal: Bulk and near net shape manufacturing processes for high-temperature, high-strength alloys are needed. Additionally, cold spray techniques can be applied in-situ at the operational level for repair and can provide multiple benefits to the nuclear industry. These tasks aim to provide information to show benefits of cold spray during the full life cycle, namely research and development, product manufacturing, and repair to mention a few key points.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2020

Investigation of Polyurethane and Fire-Retardant Foams as a Radiological Contamination Fixatives - 20202

Fixation of radiological contamination in decommissioning and deactivation can reduce worker risk, and mitigate potentially hazardous conditions; however, nearly every marketed contamination fixative has been found to be flammable, a significant concern in radiological facilities. Coupled with this, industry fixatives are normally used as a thin coating which can present problems when attempting to stabilize irregular void spaces or areas that are difficult to access and ensure full coverage. To this end, Savannah River National Laboratory (SRNL), in conjunction with Florida International University (FIU), have begun investigating the applicability of polyurethane based foaming materials, which will expand to fill a given asymmetric volume and provide fire retardancy to ensure no release of contamination in the event of a facility fire. Commercial foams undergo exothermic reactions resulting in gaseous release that subsequently causes the curing foam material to expand. Heat generation during curing can potentially compromise rubber parts of an enclosure, a significant concern in nuclear facilities. To mitigate large body heat generation, SRNL has also examined multiple layering of the material to ensure compatibility of the curing material with a previously cured body of the same material. Environmental studies were also completed in order to determine the influence on polyurethane based foams curing process. These studies showed that nearly half of the materials tested delaminated from a cured body of the same material, a property not discussed in commercially available documentation on the products. Of note was the compatibility of the foaming material with the substrate, depending on the type material that the foam was cured in/on, significant delamination could occur. Mechanical testing via tensile pull tester, dynamic mechanical analysis (DMA), and thermogravimetric analysis (TGA) was also performed. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Synthesis of Yttrium Oxide Particles for Interfacial Water Radiolysis Studies

Radiolysis of water produces hydrogen gas (H2), posing safety issues for nuclear reactors. Metal oxides can impact H2 formation when water is present on metal oxide surfaces. This presentation focuses on the development of a controllable synthesis of spherical yttrium oxide (Y2O3), that later will be tested for H2 production in water radiolysis. Y2O3 was synthesized via hydrothermal hydrolysis precipitation to form yttrium hydroxide (Y(OH)3), followed by high temperature decomposition to form Y2O3. Various synthesis conditions were tested to determine their impact on particle morphology including reaction time, cooling rate, reactant concentration, and inert atmospheres. Through short reaction times and rapid cooling rate, spherical, relatively uniform particles of 350 nm were obtained. Despite inert atmospheres, carbonate formation occurred in all particles. A calcination temperature of 800°C is necessary to remove impurities. Future work will aim to reduce carbonate formation and improve particle uniformity. The synthetic procedure will be translated to other metal ions to study their impact on interfacial radiolysis.

08 - HYDROGEN↗

DOE OSTI2020

Deconstructing the Nuclear Supply Chain Cyber-Attack Surface

The nuclear supply chain cyber-attack surface is a large, complex network of interconnected stakeholders and activities. The global economy has widened and deepened the supply chain resulting in larger numbers of geographically dispersed locations and increased difficulty ensuring the authenticity and security of digital assets. Although the nuclear industry has made significant strides in securing facilities from cyber-attacks, the supply chain remains vulnerable. This paper provides further details on each of the elements in the Digital I&C System Supply Chain Cyber-Attack Surface, including supply chain lifecycle activities, key stakeholders, touchpoints, and attack types. Deconstructing this attack surface provides insights into supply chain threats, vulnerabilities, and consequences. These insights will lead to improvements in cybersecurity supply chain risk analysis, development of new cybersecurity supply chain processes and tools, and enhancement of overall supply chain resilience.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2020

Pulsed Thermal Tomography Nondestructive Examination of Additively Manufactured Reactor Materials (Second Annual Progress Report)

Additive manufacturing (AM) is an emerging method for cost-efficient fabrication of nuclear reactor parts. AM of metallic structures for nuclear energy applications is currently based on laser powder bed fusion (LPBF) process, which can introduce internal material flaws, such as pores and anisotropy. Integrity of AM structures needs to be evaluated nondestructively because material flaws could lead to premature failures due to exposure to high temperature, radiation and corrosive environment in a nuclear reactor. Thermal tomography (TT) provides a capability for non-destructive evaluation of sub-surface defects in arbitrary size structures. Thermal tomography is a computational method for heat diffusion-based imaging of solids, which provides 3D visualization of data from flash thermography measurements. We investigate thermal tomography imaging and nondestructive evaluation of stainless steel and nickel super alloy metallic structures produced with laser powder bed fusion (LPBF) additive manufacturing (AM) process. Metallic structures produced with LPBF contain defects, and there are limited capabilities to evaluate these structures non-destructively. Thermal tomography reconstruction of 3D apparent spatial effusivity provides information about AM structure geometry and internal material flaws. We study performance of thermal tomography in imaging of metallic structures through COMSOL computer simulations of transient heat transfer, and through reconstruction of data obtained from experimental measurements. Reconstruction of internal defects is investigated using a stainless steel 316L specimen with flat bottom hole (FBH) indentations, and Inconel 718 plate produced with laser powder bed fusion (LPBF) method, which contains imprinted hemispherical shape low density regions containing non-sintered metallic powder. The FBH’s have the same sizes as the imprinted defects in the LPBF specimens, but offer better imaging contrast. Thermal tomography reconstructions provide visualizations of internal defects, and allow for estimation of their sizes and locations. Detection sensitivity of TT is limited by noises. We investigate separation of signal from noise in thermography images using several machine learning (ML) methods, including new spatio-temporal blind source separation (STBSS) and spatio-temporal sparse dictionary learning (STSDL) methods. Performance of the ML methods is benchmarked using thermography data obtained from imaging stainless steel 316L and Inconel 718 specimens produced LPBF method with imprinted calibrated porosity defects. The ML methods are ranked by F-score and execution runtime. Finally, we investigate TT of AM stainless steel 316L specimen with imprinted internal porosity defects using relatively low-cost, small form factor infrared (IR) camera based on uncooled micro bolometer detector. Sparse coding related K-means singular value decomposition (SVD) machine learning, image processing algorithms are developed to improve quality of TT images through removal of Additive white Gaussian noise without blurring the images. Following initial qualification of an AM component for deployment in a nuclear reactor, a compact TT can also be used for in-service nondestructive evaluation (NDE). With capability to perform in-service NDE of the AM component lifecycle, TT data can be used for development of a component digital twin.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2021

Aqueous-phase effects on ethanol decomposition over Ru-based catalysts

The effects of an aqueous phase on ethanol decomposition for hydrogen production over a Ru(0001) catalyst surface model have been investigated from first principles. Solvent effects on the reaction mechanism and kinetic parameters have been quantified with the help of a microkinetic reactor model, density functional theory, and an implicit solvation scheme (iSMS). Our calculations indicate that in both vapor- and aqueous-phase reaction environments, the ethanol decomposition starts with acetaldehyde formation on the surface, some of which further dehydrogenates to ketenyl species (CHCO), where the C–C bond cleaves to form methylidyne (CH) and CO. In the vapor phase, adsorbed CH gets hydrogenated to methane, and CO desorbs or undergoes methanation reducing the amount of hydrogen produced. In contrast, under aqueous phase reaction conditions, the methanation is inhibited, and the water–gas shift (WGS) reaction is accelerated, leading to complete conversion of CO to CO 2 and H 2 . Furthermore, calculations indicate that the observed reaction behavior under aqueous phase reforming conditions originates primarily from the higher water chemical potential, and implicit solvent models predict only a small solvation effect.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

A new perspective on density and strength loss profiles at the surface of thermally oxidized nuclear graphite

Oxidation of graphite components could influence their designed life in a high-temperature nuclear reactor. The oxidized regions could potentially lower the allowed stress capacity. The American Society of Mechanical Engineers rules for the design and construction of graphite-moderated reactors recommend that subsurface regions that might become excessively damaged by oxidation during reactor operation be identified and excluded from geometry and stress calculations. Identification of oxidation-affected regions is possible, in principle, through complex modeling exercises of reactor behavior during hypothetical accident scenarios coupled with graphite oxidation models, but this procedure may not have the precision needed for informed decisions. Here, this paper proposes an alternate method, based on interpretation of a series of well-designed oxidation experiments, which could augment the designer's tools. The procedure is illustrated by data on oxidation by air of several graphite grades (NBG-18, PCEA, IG-110, R4-650) that are corroborated with independent literature information, when available. The Wichner model for graphite oxidation used for this analysis provides conservative results that could be quickly implemented in the design process.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Be Surface Structures on W(110) and W(211): A DFT Study

Beryllium and Tungsten are promising candidates for use as plasma facing materials (PFMs) in upcoming fusion reactors. Many complex and competing phenomena however complicate the understanding and development of materials that operate in the harsh conditions of the reactor. In particular, redeposition of Be onto the W divertor must be considered due to the expected erosion of the Be first wall under exposure to the plasma. It is known that a build up of Be on W allows for the formation of BeW alloys which can harm the longevity and performance of the fusion divertor. In an effort to understand the interaction of Be with W surfaces, a study of Be structures on W(110) and W(211) as a function of Be coverage has been carried out using Density Functional Theory. We have found that both W surfaces develop monolayers of Be characterized by a densely packed hexagonal structure. Below this monolayer coverage, Be structures are found to have two motifs of coverage, a densely packed hexagonal pattern punctuated by areas of low-density coverage. The structures found here produce work function values and trends in good agreement with experimental measurements.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Inductively Coupled Nonthermal Plasma Synthesis of Size-Controlled γ-Al 2 O 3 Nanocrystals

Gamma alumina (γ-Al 2 O 3 ) is widely used as a catalyst and catalytic support due to its high specific surface area and porosity. However, synthesis of γ-Al 2 O 3 nanocrystals is often a complicated process requiring high temperatures or additional post-synthetic steps. Here, we report a single-step synthesis of size-controlled and monodisperse, facetted γ-Al 2 O 3 nanocrystals in an inductively coupled nonthermal plasma reactor using trimethylaluminum and oxygen as precursors. Under optimized conditions, we observed phase-pure, cuboctahedral γ-Al 2 O 3 nanocrystals with defined surface facets. Nuclear magnetic resonance studies revealed that nanocrystal surfaces are populated with AlO 6 , AlO 5 and AlO 4 units with clusters of hydroxyl groups. Nanocrystal size tuning was achieved by varying the total reactor pressure yielding particles as small as 3.5 nm, below the predicted thermodynamic stability limit for γ-Al 2 O 3 .

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2022

A low-input strategy for chromium removal from industrial stormwater using peat sorbent

Low-cost and low-input water treatment systems are important for industrial stormwater remediation. Here we examine a flow-through reactor treatment installation where water exceeds the allowable maximum concentration for drinking water in multiple metals (e.g., chromium [Cr], cadmium [Cd], zinc [Zn]) prior to treatment. Specifically, we seek to understand why Cr attenuated in the reactors is not leachable by identifying the specific chemical form of Cr and dominant mechanisms promoting sequestration in the reactors. Total solid-phase Cr concentration in the peat media ranged from 50 to 150 mg/kg after 1 yr of exposure to stormwater to 300 to 900 mg/kg after 3.5 yr. X-ray fluorescence mapping images show Cr, iron (Fe), and Zn spatially correlated over a scale of 10 μm to 5 mm. Chromium rinds form on the edges of peat particles as Cr accumulates. Chromium and Fe K-edge X-ray absorption near edge structure spectroscopy reveal chromium predominately in the 3+ oxidation state with lesser amounts of elemental Cr. We propose the primary means of chromium attenuation in the reactors is precipitation as Cr-Fe hydroxides combined with trivalent Cr adsorption onto peat surfaces.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Effect of CO on alcohol oxidation over commercial oxidation catalysts for control of emissions from lean-burn engines

For commercialization, alcohol-based net-zero carbon fuels in diesel-driven internal combustion engines must meet emissions standards set by the U.S. Environmental Protection Agency. Here, a series of aged commercial oxidation catalysts, Pt diesel oxidation catalyst (DOC), Pd+Pt DOC, and Pt oxidation catalyst (Pt OC), were studied using an automated flow reactor and in situ DRIFTS techniques to investigate the impact of CO on alcohol oxidation. Surface formate and acetate intermediates were formed due to partial oxidation of methanol and ethanol, respectively. Sequential introduction of alcohol and CO experiments using in situ DRIFTS on all three catalysts showed that CO inhibited low temperature methanol oxidation. Mutual inhibition effects between CO and ethanol were observed during co-oxidation. Acetate species shifted CO oxidation to higher temperatures on Pt DOC and Pt OC, whereas CO pre-exposure inhibited acetate formation. CO oxidation occurred at lower temperatures during ethanol and CO co-oxidation on Pd+Pt DOC.

33 ADVANCED PROPULSION SYSTEMS↗

DOE OSTI2024

Bayesian parameter estimation and evaluation of the K -ω shear stress transport model for plane impinging jets

Numerical simulations with semi-empirical turbulence models are commonly used to model impinging jets, often used for cooling solid surfaces. In this work, the constants in the k-ω shear stress transport model in ANSYS FLUENT are calibrated to experimental velocity and heat transfer data for a plane turbulent impinging air jet to determine if Kennedy-O'Hagan calibration (Kennedy and O'Hagan 2001 J. R. Stat. Soc. B 63 425–64) can improve predictions of near-surface velocities and surface Nusselt numbers for similar flows. Impinging jets have been proposed to cool the target plates of the divertor in future magnetic fusion energy reactors, where simulations are used to estimate divertor performance. The flat-plate divertor (Wang et al 2009 Fusion Sci. Technol .56 1023–7) uses a plane jet of helium issuing from a B = 0.5 mm slot to cool a surface with radius of curvature of 44 B at a distance 4 B from the slot. Predictions from the calibrated numerical model are compared with independent experimental data at different flow conditions, as well as surface temperature data for a flat plate divertor test section. The contribution of this work is evaluation of the accuracy of a calibrated turbulence model for modest extrapolations in flow geometry and flow conditions for a plane impinging jet.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2022

Additive manufacturing of complex objects using refractory matrix materials

A method for the manufacture of a three-dimensional object using a refractory matrix material is provided. The method includes the additive manufacture of a green body from a powder-based refractory matrix material followed by densification via chemical vapor infiltration (CVI). The refractory matrix material can be a refractory ceramic (e.g., silicon carbide, zirconium carbide, or graphite) or a refractory metal (e.g., molybdenum or tungsten). In one embodiment, the matrix material is deposited according to a binder-jet printing process to produce a green body having a complex geometry. The CVI process increases its density, provides a hermetic seal, and yields an object with mechanical integrity. The residual binder content dissociates and is removed from the green body prior to the start of the CVI process as temperatures increase in the CVI reactor. The CVI process selective deposits a fully dense coating on all internal and external surfaces of the finished object.

Terrani, Kurt A.↗

DOE OSTI2024

Additive manufacturing of complex objects using refractory matrix materials

Terrani, Kurt A.↗

DOE OSTI2026

Synergistic Solvent-Surface Interactions Enable Alkyne Semihydrogenation at Palladium

Enabling higher yield and better selectivity for fine-chemical synthesis through heterogeneous catalysis is intricately linked to the interplay of active sites, reaction conditions, and mass transfer influence provided by the catalyst. Alkyne semihydrogenation is ubiquitous in the production of bulk chemicals in the pharmaceutical, polymer, or fine-chemical industries, but product selectivity remains a major challenge. Here, in this study, we demonstrate that the design of catalysts encompassing nickel (Ni) foams as contiguous monolith supports, decorated with ultralow loading of Pd/PdO x nanoparticles on a carbonized polydopamine interface and tuned with a thin layer of Al 2 O 3 , in conjunction with an optimized reaction environment leads to highly selective alkyne semihydrogenation. The reactions demonstrate good functional group tolerance and applicability to flow reactor systems. Combined computational and experimental studies are presented to describe the synergistic effect between the solvent-surface interaction and the degree of Pd surface reduction that are necessary to promote this selectivity. The system highlights the opportunity for catalyst-solvent codesign as a benign alternative to more complex reactants featuring extrinsic poisons or less-favored dopants.

atomic layer deposition↗