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Synthesis, Processing and Properties of Calcium- and Nickel-Doped Yttrium Chromates(III) Y{sub 0.8}Ca{sub 0.2}Cr{sub 1−x}Ni{sub x}O{sub 3} (x = 0-0.3) and Studies on Their Potential Application as Coatings for SOFC Interconnects

In the present study, a calcium- and nickel-doped yttrium chromates (YCCN)-based, conductive–protective layers for metallic interconnects used in the intermediate-temperature solid oxide fuel cells (IT-SOFCs) were investigated. Synthesis of Y{sub 0.8}Ca{sub 0.2}Cr{sub 1−x}Ni{sub x}O{sub 3} (x = 0; 0.15 and 0.3) powders was performed using a wet chemistry method with two different complexing agents: ethylenediaminetetraacetic acid and glycine. Based on the result of thermal analysis of obtained precursors, optimal conditions of the calcination process were determined. Powders were then milled, compacted and sintered at different temperatures using free sintering method, into series of dense, polycrystalline sinters. The use of glycine precursor allowed obtaining a single-phase material in all cases. Based on the electrical and sintering properties, the Y{sub 0.8}Ca{sub 0.2}Cr{sub 0.85}Ni{sub 0.15}O{sub 3} material was selected for further studies. It was deposited using cost-effective screen-printing method on the Crofer 22APU ferritic stainless steel. To investigate properties and suitability of the resulting layer/steel system for IT-SOFCs applications, the high-temperature, dual-atmosphere studies were carried out for the first time for ceramic/metallic system, in conditions as close as possible to actual working conditions of the fuel cell. The layer exhibited high stability and good protective properties. The area-specific resistance of the studied ceramic layer/metallic substrate composite was determined, with the obtained value of 0.0366 Ω cm{sup 2} being within the arbitrary limit set for these materials (0.1 Ω cm{sup 2}). The results show that the investigated materials are suitable for the projected application.

36 MATERIALS SCIENCE↗

Interface Reactions Responsible for Run-Out in Active Brazing: Part 1

The run-out phenomenon was observed in Ag-Cu-Zr active braze joints made between the alumina ceramic and Kovar™ base material. Run-out introduces a significant yield loss by generating functional and/or cosmetic defects in brazements. A prior study identified a correlation between run-out and the aluminum (Al) released by the reduction/oxidation and the latter’s reaction with the Kovar™ base material. A study was undertaken to understand the fundamental principles of run-out by examining the interface reaction between Ag-xAl filler metals (x=2, 5, and 10 wt.%) and Kovar™ base material. Sessile drop samples were fabricated using brazing temperatures of 965°C or 995°C and times of 5 min or 20 min. The correlation was made between the degree of wetting-and-spreading by the sessile drops and the run-out phenomenon. Wetting-and-spreading increased with Al content (x) of the Ag-xAl filler metal, but was largely insensitive to the brazing process parameters. The increased Al concentration resulted in higher Al contents of the (Fe, Ni, Co) x Al y reaction layer. Run-out was predicted when the filler metal has a locally-elevated, Al content exceeding 2 – 5 wt.%. Lastly, several mitigation strategies were proposed, based upon these findings.

36 MATERIALS SCIENCE↗

Detection Of Special Nuclear Materials Tagged Neutrons

In order to detect Special Nuclear Materials (SNM) in unattended luggage or cargo containers in the field of homeland security, fissions are induced by 14 MeV neutrons produced by an associated particle DT neutron generator, and prompt fission particles correlated with tagged neutron are detected by plastic scintillators. SMN produce high multiplicity events due to induced fissions, whereas nonnuclear materials produce low multiplicity events due to cross-talk, (n,2n) or (n,n'γ) reactions. The data acquisition electronics is made of compact FPGA boards. The coincidence window is triggered by the alpha particle detection, allowing to tag the emission date and direction of the 14 MeV interrogating neutron. The first part of the paper presents experiment vs. calculation comparisons to validate MCNP-PoliMi simulations and the post-processing tools developed with the data analysis framework ROOT. Measurements have been performed using different targets (iron, lead, graphite), first with small plastic scintillators (10 x 10 x 10 cm{sup 3}) and then with large detectors (10 x 10 x 100 cm{sup 3}) to demonstrate that nuclear materials can be differentiated from nonnuclear dense materials (iron, lead) in iron and wood matrixes. A special attention is paid on SNM detection in abandoned luggage. In the second part of the paper, the performances of a cargo container inspection system are studied by numerical simulation, following previous work reported in. Detectors dimensions and shielding against the neutron generator background are optimized for container inspection. Events not correlated to an alpha particle (uncorrelated background), counting statistics, time and energy resolutions of the data acquisition system are all taken into account in a realistic numerical model. The impact of the container matrix (iron, ceramic, wood) has been investigated by studying the system capability to detect a few kilograms of SNM in different positions in the cargo container, within 10 min acquisitions. (authors)

36 MATERIALS SCIENCE↗

Cross-flow separation characteristics and piloting of graphene oxide nanofiltration membrane sheets and tubes for kraft black liquor concentration

Dewatering of weak black liquor (WBL) in the kraft cycle by evaporation is highly energy intensive. Membranes are an attractive alternative for energy-efficient dewatering, but existing commercial polymeric or ceramic membranes are either degraded in BL or have high capital costs. Our recent works have demonstrated the engineering of graphene oxide (GO) nanofiltration membranes, their stability and promising performance in BL conditions, and preliminary scale-up into sheets and tubes. Here, we describe in detail the separation characteristics of GO membrane sheets and tubes under real BL conditions and crossflow operation. Recycle-mode piloting of a GO tubular membrane showed average “production flux” of 16 L/m2/h (LMH) and high rejections of lignin (98.3%), total solids (66%), and total organic carbon (83%), with no signs of irreversible fouling identified. A corresponding GO sheet membrane produced an average flux of ~25 LMH and maintained high lignin rejection of ~97% during a slipstream pilot at a kraft mill site using WBL with ~16 wt% total solids (TS). Finally, we piloted a Dow/DuPont XUS1808 polyamide composite reverse osmosis (RO) membrane for last-mile processing of the GO nanofiltration membrane permeate. The RO membrane showed a steady state flux of 19 LMH at 65 bar and produced ~0.02 wt% TS water product, which is highly suitable for reuse in pulp washing operations in the kraft process. The results have strong positive implications for the industrial application of GO membranes in BL concentration and other related applications.

Materials Science↗

Structure and ionic conductivity of well-aligned polycrystalline sodium titanogallate grown by reactive diffusion

We prepared the b-axis-oriented polycrystalline Na{sub 0.85}Ti{sub 0.51}Ga{sub 4.37}O{sub 8} (NTGO) embedded in Ga{sub 2}O{sub 3}-doped Na{sub 2}Ti{sub 4}O{sub 9} matrix using the reactive diffusion technique. When the sandwich-type Ga{sub 2}TiO{sub 5}/NaGaO{sub 2}/Ga{sub 2}TiO{sub 5} diffusion couple was heated at 1323 K for 24 h, the NTGO polycrystal was readily formed in the presence of a liquid phase. The resulting polycrystalline material was characterized by X-ray diffractometry, electron microscopy and impedance spectroscopy. We mechanically processed the annealed diffusion couple and obtained the thin-plate electrolyte consisting mostly of the grain-aligned NTGO polycrystal. The ionic conductivity (σ) of the electrolyte along the common b-axis direction steadily increased from 1.3×10{sup −4} to 7.3×10{sup −3} S/cm as the temperature increased from 573 to 1073 K. There was a slope change at ca. 792 K for the Arrhenius plot of σ; the activation energies were 0.39 eV above this temperature and 0.57 eV below it. The NTGO showed the crystal structure (space group C2/m) with substantial positional disordering of one of the two Ga sites. The Na{sup +} ions occupied ca. 43% of the Wyckoff position 4i site, the deficiency of which would contribute to the relatively high ionic conductivity along the b-axis. The reactive diffusion could be widely applicable as the novel technique to the preparation of grain-aligned ceramics of multi-component systems. - Graphical abstract: We have prepared the b-axis-oriented Na{sub 0.85}Ti{sub 0.51}Ga{sub 4.37}O{sub 8} polycrystal embedded in Ga{sub 2}O{sub 3}-doped Na{sub 2}Ti{sub 4}O{sub 9} matrix by the heat treatment of sandwich-type diffusion couple of Ga{sub 2}TiO{sub 5}/NaGaO{sub 2}/Ga{sub 2}TiO{sub 5}. The resulting Na{sub 0.85}Ti{sub 0.51}Ga{sub 4.37}O{sub 8} electrolyte showed the ionic conductivity ranging from 1.3×10{sup −4} S/cm at 573 K to 7.3×10{sup −3} S/cm at 1073 K. - Highlights: • The b-axis-oriented polycrystalline Na{sub 0.85}Ti{sub 0.51}Ga{sub 4.37}O{sub 8} is successfully prepared. • Crystal structure of Na{sub 0.85}Ti{sub 0.51}Ga{sub 4.37}O{sub 8} is determined by single-crystal XRD. • The polycrystal shows relatively high Na{sup +} ion conductivity along the common b-axis. • Reactive diffusion is successfully used for the preparation of grain-aligned ceramics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Optimising National WM Strategies through early consideration of Nuclear Safeguards - 18607

International Atomic Energy Agency (IAEA) safeguards stand alongside safety and security as one of the three pillars for prudent management of all nuclear material, including nuclear waste. Although safety considerations, including public and environmental radiation protection, are the traditional drivers of waste management strategies, there is a requirement for nuclear safeguards in shaping and quantifying long-term solutions for special classes of radioactive waste. This is especially important when considering the disposal of nuclear material in a repository that could be released from regulatory oversight for radiation protection after a period of institutional control, as some safeguards oversight would still be required. Failure to consider nuclear safeguards at the early stages of planning may alternatively lead to excessive volumes for disposal or the need to recondition already treated wastes. At the very least, safeguards measures should be considered before countries seek to dispose of legacy nuclear materials, decommissioning wastes and other materials containing uranium, thorium or plutonium in an operating repository. Nuclear safeguards are the set of tools and techniques used by the IAEA to verify that countries comply with their international obligations not to divert nuclear materials to nuclear explosive devices. Under the Nuclear Non-Proliferation Treaty (NPT), nuclear safeguards apply to all uranium, thorium and plutonium held in non-weapons NPT states, with limited exceptions. In nuclear-weapon states, much of their material is likewise subject to IAEA safeguards through conditions in agreements with respective suppliers of the uranium. Under IAEA safeguards, such nuclear material must remain accounted for and accessible for periodic verification-analogous to the safety concepts of reversibility and retrievability. Nevertheless, safeguards requirements can be terminated - provided that the State and the [IAEA] agree that such nuclear material is practicably irrecoverable - through dilution or immobilisation in solid form (such as cement, glass or ceramic). This means candidate material can be disposed of as non- nuclear material, with no further safeguards requirements, provided this criterion is met. Unlike radiological wastes where repository design strongly influences pathways for radionuclide migration and overall safety performance, repository design is not a factor in considering the termination of safeguards on nuclear material. This paper looks at similarities and differences in the safety, security and safeguards regulatory requirements for the management of radioactive waste and nuclear material in Australia. In particular, it outlines recent experience gained from participation in Australia's waste acceptance criteria working group for a national low-level waste repository and intermediate-level waste store, as well as from Australia's overall waste management strategy. These items of work have coincided with the IAEA update of its internal policy on termination of safeguards on nuclear material. Australia's experience shows how inclusion of safeguards criteria in the planning process is leading to optimisations in choice of facility concepts, project sequencing and equitable distribution of economic risk. By considering the three pillars-safety, security and safeguards-early on in the planning process, Australia's waste management strategy will provide a benchmark for other states in establishing and updating their own waste acceptance criteria for the disposal of nuclear material. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

An Organic, Direct Bonded Copper, Multi-Layered, Ultra-Low Inductance Package for High-Power UWBG MOSFETs

The most common metalized substrates used in high-power switching packages consist of a ceramic layer such as Aluminum Nitride (AlN) sandwiched between two copper layers. Ceramic substrates are used because it has the key characteristic of having high dielectric strength while being thermally conductive. A large drawback to ceramic substrates is that they do not allow for a multi-layered circuit design. By replacing the traditional ceramic substrate with organic direct bonded copper (ODBC) we can open a wide range of possibilities when it comes to power module layout such as multi-layered circuits and double-sided cooling. Both benefits are critical while packaging high-performance Gallium Oxide (Ga2O3) MOSFETs. Because of Ga2O3's relatively poor thermal conductivity, a double-sided cooled package becomes necessary. Therefore, the use of ODBC provides the flexibility to fabricate copper traces carrying much higher currents, and by creating a multi-layered package, we can drastically reduce the parasitic inductance inside the power module. Achieving lower parasitic inductance is critical for an ultra-fast Ga2O3 package to avoid excessive voltage overshoot and ringing. Using ODBC, we have designed novel packages capable of handling the challenges presented by fast Ga2O3 switching. Using multi-physics modeling software, we can validate our design before building the prototype. Due to the simple process parameters needed to work with ODBC, we can rapidly create prototypes without using external vendors. This flexibility allows us to quickly design, build, and validate highly complex switching power modules to accommodate next generation, Ga2O3 switching devices.

ADVANCED PROPULSION SYSTEMS,ENGINEERING↗

RF sheath induced sputtering on Proto-MPEX. I. Sheath equivalent dielectric layer for modeling the RF sheath

The pulsed linear plasma device Prototype Material Plasma Exposure eXperiment (Proto-MPEX) uses a radio frequency (RF) helicon antenna with an aluminum nitride ceramic window for plasma production. The RF sheath created under the helicon antenna is sufficient to cause ion impact energies to be greater than the sputtering threshold of the AlN helicon window material and for impurities to be created. In this study, we investigate the RF sheath on the inner diameter of the helicon window and its impact on the impurity production rates in Proto-MPEX. Three models—a 3D COMSOL finite element RF model of the Proto-MPEX helicon region, a rectified DC sheath potential model, and the 3D Global Impurity TRansport code—are coupled together to study impurity production and transportation. This novel method of impurity generation and transport modeling spans length scales ranging from the sheath (millimeters or less) up to the full device (meters) and can be applied to other radio frequency sources and antennas in a wide range of plasma physics studies, including basic plasmas, low-temperature processing plasmas, plasma thrusters, and fusion plasmas.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Narrow-Channel, Fluidized Beds for Effective Particle Thermal Energy Transport and Storage

Colorado School of Mines (Mines) led this program in collaboration with Sandia National Laboratories (Sandia) to characterize narrow-channel fluidized beds of aluminosilicate particles – supplied by Carbo Ceramics – as a means for releasing high-temperature thermal energy in particle heat exchangers and for capturing concentrated solar energy in indirect particle receivers. Single-channel, heat transfer experiments at Mines and reduced-order 1-D models and 3-D two-fluid, CFD models explored many aspects of counterflow, bubbling fluidized beds (net downward particle flow and upward gas flow) for enhancing particle-wall heat transfer at elevated temperatures. Results at Mines on single-channel test sections consistently showed that mild bubbling fluidization increases particle-wall heat transfer coefficients (h T,w ) regularly by more than 4.0x over h T,w values without fluidization at similar conditions (mean particle diameter d p , bed depth Δz b , and bed particle temperatures T p ). Insights from lab-scale tests and modeling studies provided Nusselt number correlations for h T,w and informed the design and fabrication (by Vacuum Process Engineering) of a nominal 40-kWth, particle-sCO 2 plate heat exchanger (HX) with 12 parallel narrow-channel, fluidized beds bounded by stainless-steel walls with embedded microchannels for high-pressure sCO 2 flows. Tests of the 40-kW th HX at the particle-sCO 2 HX test stand at Sandia's National Solar Thermal Test Facility (NSTTF) were limited, due to HX design, to particle inlet temperatures T p,in ≤ 520°C with maximum sCO 2 outlet temperatures T sCO2,out ≈ 440°C, which are well below design conditions for a primary HX in a sCO 2 power cycle for a Gen-3 concentrating solar power (CSP) plant. Total heat transfer $\dot{Q}_{HX}$ remains relatively constant with increased fluidization for fixed particle and sCO 2 inlet conditions because higher h T,w due to fluidization is offset by increased axial dispersion, which suppresses temperature differences between the particles and sCO 2 in the counterflow configuration. The axial dispersion reduces the effective overall heat transfer coefficient U based on T p,in to values around 200 W m -2 K -1 .

14 SOLAR ENERGY↗

Additive manufacturing of complex-shaped graded TiC/steel composites

Complex-shaped TiCx ceramic preforms with a gradient of carbon content in the titanium carbide phase (x changes from 0.7 to 0.98) were fabricated for the first time by Binder jet 3D printing technology. The complex-shaped preforms were infiltrated with molten carbon steel (0.7 wt.%C). Thermodynamic considerations showed that carbon could be transferred from titanium carbide to steel and vice versa according to the initial concentration of carbon (activity) in both phases. After infiltration, solidification and slow cooling, a microstructural gradient was obtained throughout the steel matrix from ferrite, in the region where the steel was in contact with titanium carbide of low carbon content (x=0.7), to pearlite, in the region where the steel underwent interactions with stoichiometric titanium carbide (x=0.98). After annealing at 900°C and quenching in oil, a structural gradient in the steel matrix from ferrite to martensite was obtained, resulting in a hardness gradient of 700-1600 HV. The suggested processing approach allows for fabrication of complex-shaped graded composites with the desired property gradient suitable for a wide range of practical applications.

36 MATERIALS SCIENCE↗

Low-Cost Radiant Heater for Rapid Response, High-Temperature Heating

High-temperature processing has an irreplaceable role in many research and industrial applications. Despite remarkable development spanning over a century, the pursuit of even higher thermal flux density and more rapid thermal transients has not slowed down. As part of the ongoing energy evolution, many industrial applications are transitioning from direct combustion of fossil fuels as primary energy sources to increasing electrification, capable of adapting to renewable power grids. Thus, there is an emerging need for electrical heaters that can replace burners and supply the heat demand, especially at the highest temperatures. In this study, we report on a radiant heater design that can achieve cyclic heating/cooling rates of up to 400 K min –1 and a temperature range in excess of 1,800 K, comparable to those of commercial infrared gold image furnaces, at high surface and volumetric power densities. The heater consists of a modular unit of incandescent tungsten filament and is enclosed in an evacuated ceramic envelope, chemically inert, tolerant of thermal shock, and impervious to gasses. The material and manufacture cost of such heaters, which is estimated at ~$0.05/W, is less than 0.03% of that for infrared gold image furnaces, which is at >$2/W. Tests of more than 10,000 demanding cycles (high temperature and high heating/cooling rate) over 350 h of total operational time and in different temperature ranges confirm the robust performance of radiant heater prototypes. The design is widely applicable to high-temperature reactor and furnace designs. In thermochemistry research and practice, these radiant heaters could offer multiple benefits compared to solar simulators, lasers, infrared gold furnaces, ceramic heaters, or direct concentration of solar input.

99 GENERAL AND MISCELLANEOUS↗

Designing Glass and Crystalline Phases of Metal–Bis(acetamide) Networks to Promote High Optical Contrast

Owing to their high tunability and predictable structures, metal–organic materials offer a powerful platform to study glass formation and crystallization processes and to design glasses with unique properties. In this work, we report a novel series of glass-forming metal–ethylenebis(acetamide) networks that undergo reversible glass and crystallization transitions below 200 °C. The glass-transition temperatures, crystallization kinetics, and glass stability of these materials are readily tunable, either by synthetic modification or by liquid-phase blending, to form binary glasses. Pair distribution function (PDF) analysis reveals extended structural correlations in both single and binary metal–bis(acetamide) glasses and highlights the important role of metal–metal correlations during structural evolution across glass–crystal transitions. Notably, the glass and crystalline phases of a Co–ethylenebis(acetamide) binary network feature a large reflectivity contrast ratio of 4.8 that results from changes in the local coordination environment around Co centers. These results provide new insights into glass–crystal transitions in metal–organic materials and have exciting implications for optical switching, rewritable data storage, and functional glass ceramics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Understanding the structure and mechanism of Na + diffusion in NASICON solid-state electrolytes and the effect of Sc- and Al/Y-substitution

NASICON (sodium superionic conductor) based ceramics are one of the most promising classes of solid-state electrolytes for all-solid-state batteries. However, the mechanism of sodium ion diffusion is not understood in great detail since there is still a discrepancy between reported average structure models, local structures, and the number and position of sodium sites. To close this gap, we investigate the underlying diffusion mechanism and structural changes governing the Na + transport in Na 3.4 Zr 2 Si 2.4 P 0.6 O 12 using quasielastic neutron scattering (QENS) and powder X-ray diffraction (XRD). In the temperature range from 298 K to 640 K, the correlations between structural changes of a monoclinic C2/c to rhombohedral R $\bar{3}$c phase transition and the result of ion diffusion are investigated. The analysis of the quasielastic neutron scattering data reveals two quasielastic components corresponding to the Chudley-Elliott jump-diffusion model. It clearly shows two different Na + diffusion processes, local and long-range, on two different time and length scales and allows calculations of their corresponding activation energies. Additionally, the effects of Sc 3+ and Al 3+ /Y 3+ aliovalent substitution of Zr 4+ ions on the crystal structure and Na + diffusion are also studied. We can distinguish a local, chain, and cross-chain diffusion mechanism based on correlated QENS and XRD comparison of relevant nearest crystallographic Na–Na distances. The results reveal that the Na + diffusion in these NASICONs is three-dimensional and can provide guidelines on how dopants and changes in the crystal structure can affect the Na + conductivity.

25 ENERGY STORAGE↗

Nanoplastic removal function and the mechanical nature of colloidal silica slurry polishing

The nanomechanical deformations on a broad range of optical material surfaces (single crystals of Al 2 O 3 [sapphire], SiC, Y 3 Al 5 O 12 [YAG], CaF 2 , and LiB 3 O 5 [LBO]; a SiO 2 –Al 2 O 3 –P 2 O 5 –Li 2 O glass-ceramics [Zerodur]; and glasses of SiO 2 :TiO 2 [ULE], SiO 2 [fused silica], and P 2 O 5 –Al 2 O 3 –K 2 O–BaO [Phosphate]) near the elastic-plastic load boundary have been measured by nanoindentation and nanoscratching to mimic the nanoplastic removal caused by a single slurry particle during polishing. Nanoindenation in air was performed to determine the workpiece hardness at various loads using a commercial nanoindenter with a Berkovich tip. Similarly, an atomic force microscope (AFM) with a stiff diamond coated tip (150 nm radius) was used to produce nanoplastic scratches in air and aqueous environments over a range of applied loads (~20-170 μN). The resulting nanoplastic deformation of the nanoscratches were used to calculate the removal function (i.e., depth per pass) which ranged from 0.18 to 3.6 nm per pass for these materials. A linear correlation between the nanoplastic removal function and the polishing rate (using a fixed polishing process with colloidal silica slurry on a polyurethane pad) of these materials was observed implying that: (a) the polishing mechanism using colloidal silica slurry can be dominated by mechanical rather than chemical interactions; and (b) the nanoplastic removal function, as opposed to interface particle interactions, is the controlling factor for the polishing material removal rate. Furthermore, this correlation is consistent with the Ensemble Hertzian Multi-Gap (EHMG) microscopic material removal rate model described previously. The nanoplastic removal depth was also found to correlate to the measured nanoindentation hardness (H1) of the optical material, scaling as H 1 -3.5 . Two-dimensional (2D) finite element analysis simulations of nanoindentation showed a similar nonlinear dependence of plastic deformation with the workpiece material hardness. The findings of this study are used to determine an effective Preston coefficient for the material removal rate expression and enhance the predictive nature of the nanoplastic polishing rate for various materials utilizing their material properties.

36 MATERIALS SCIENCE↗

Evaluation of Binder Jetting and Chemical Vapor Infiltration as a Production Method for Silicon Carbide Parts for Nuclear Applications

Application of silicon carbide (SiC) is often sought within nuclear energy systems due to its high thermal conductivity, mechanical and environmental stability at elevated temperatures, corrosion resistance, and exceptional displacement damage irradiation tolerance. As such, the transformational challenge reactor (TCR) program is considering its application in its additively manufactured core. SiC may be used as the matrix for the TCR fuel blocks that comprise of TRISO fuel particles embedded inside this material or used as core non-fuel-bearing peripherical structures such as bottom support manifolds. The core peripherical structures serves to support the overall core geometry, direct and guide coolant flow, and also reflect back leaked neutrons into the core. SiC has very low neutron absorption and adequate scattering cross sections that makes it an ideal material for utilization in the TCR core. Like many ceramics, however, SiC is difficult and at times impractical to shape into complex geometries via traditional machining due to its brittleness. Further, large structures comprising nuclear-grade SiC, i.e. highly pure and crystalline, are costly. Additive manufacturing (AM), however, offers the ability to shape materials by adding layer-by-layer rather than subtracting, contributing new possibilities for previously difficult-to-shape materials. Thus, exploring AM as a method to shape SiC offers a highly cost-effective method and is strategic to developing the next generation of components for nuclear reactors. This report outlines an evaluation of binder jet additive manufacturing combined with chemical vapor infiltration (CVI) to produce nearly-dense silicon carbide artifacts in complex geometries suitable for advanced nuclear reactor designs. The focus is placed on the binder jet printing technologies at large scale for nonfuel-bearing structures relevant to the TCR core and other advanced reactors. Among all AM processes, binder jet delivers the highest resolution capability while still maintaining large print sizes, making it the ideal candidate for nuclear component production.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Detecting damage in composites using volume decomposition analysis of tomographic data

Detection of damage in a single tow ceramic matrix composite specimen has been achieved using orthogonal decomposition of volumetric tomographic datasets collected at four tensile loads. This decomposition approach has been applied at two different length scales: (i) individual fibres and (ii) bulk volumes containing fibres and matrix material. Volumes were first decomposed to feature vectors, orders of magnitude smaller than the original volume they describe, and then comparisons between datasets at different load levels were made in feature vector space. The results show quantitative measurements of damage location, damage morphology and the relative growth of this damage with increased load when compared with a dataset with less or no damage. No prior knowledge of the dataset or training of algorithms is required for damage to be detected, it is only necessary that at least two datasets are available for comparison, e.g. from in situ or repeated scanning measurements. Results are generated on significantly shorter timescales when compared with previous automated approaches to tomography data processing. This approach has the potential to be applied to damage detection in a range of materials through comparisons of volumetric datasets from a range of measurement or computational techniques.

Middleton, Ceri A.↗

Role of electronic energy loss on defect production and interface stability: Comparison between ceramic materials and high-entropy alloys

High-entropy alloys (HEAs) and some complex alloys exhibit desirable properties and significant structural stability in harsh environments, including possible applications in advanced reactors. Energetic ion irradiation is often used as a surrogate for neutron irradiation; however, the impact of ion electronic energy deposition and dissipation is often neglected. Moreover, differences in recoil energy spectrum and density of cascade events on damage evolution must also be considered. In many chemically complex alloys, the mean free path of electrons is reduced significantly, thus their decreased thermal conductivity and slow dissipation of localized radiation energy can have noticeable effects on displacement cascade evolution that is greatly different from metals with high thermal conductivity. In this work, nanocrystalline HEAs of Ni 20 Fe 20 Co 20 Cr 20 Cu 20 and nonequiatomic (NiFeCoCr) 97 Cu 3 , both having much lower room-temperature thermal conductivity than pure Ni or Fe, are chosen as model HEAs to reveal the role that electronic energy loss during ion irradiation has in complex alloys. The response of nanocrystalline HEAs is investigated under irradiation at room temperature using MeV Ni and Au ions that have different ratios of electronic energy to damage energy, which is the energy dissipated in displacing atoms. Different from previously reported amorphization of nanocrystalline SiC, experimental results on these HEAs show that, similar to the process in nanocrystalline oxide materials, both inelastic thermal spikes via electron–phonon coupling and elastic thermal spikes via collisions among atomic nuclei contribute to the overall grain growth. The growth follows a power law dependence with the total deposited ion energy, and the derived value of the power-exponent suggests that the irradiation-induced instability at and near grain boundaries leads to local rapid atomic rearrangements and consequently grain growth. The high power-exponent value can be attributed to the sluggish diffusion and delayed defect evolution arising from the chemical complexity intrinsic to HEAs. Here, this work calls attention to quantified fundamental understanding of radiation damage processes beyond that of simplified displacement events, especially in simulating neutron environments.

36 MATERIALS SCIENCE↗

Nano-Engineered Catalyst Supported on Ceramic Hollow Fibers for the Utilization of CO 2 in Dry Reforming to Produce Syngas

The objective of this project was to develop a novel catalytic reactor containing nano-engineered catalysts for the utilization of CO 2 (captured from coal-fired power plants and other CO 2 emitting sources) in dry methane reforming (DMR) (CO 2 + CH 4 → 2 H 2 + 2 CO) to produce synthesis gas (syngas). The technology aims to reduce CO2 emissions by developing beneficial uses for CO 2 from coal-fired power plants. It also offers an alternative to mitigate CO 2 emissions in areas where geologic storage may not be an optimal solution and/or utilization could significantly offset the costs of carbon capture and sequestration. The nano-engineered Ni-based catalyst was prepared by atomic layer deposition (ALD). The Ni particles were as small as ~2-4 nm. The nano-engineered catalyst showed CH 4 conversion >95%, H 2 /CO ratio in the range of 0.7-1.0, and CH 4 reforming rate as high as 2,500 L/h/gNi at 850 ºC and pressure of 15-25 psia. The Ni-based ALD catalyst also showed good stability in DMR reaction during a 200-h continuous operation at 850 °C. This is due to strong bonding between the nanoparticles and substrates since the Ni nanoparticles were chemically bonded to the substrate during the ALD process. The high thermal stability maintains the high dispersion of Ni nanoparticles, which can inhibit coke formation because their step edges are small enough to limit carbon nucleation and growth. Technoeconomic analysis (TEA) indicates the levelized cost of syngas (LCOS) is $172/ton with our technology, which is lower than the equivalent (molar) cost of hydrogen produced by steam methane reforming (SMR) or autothermal reforming (ATR). The major operating cost is natural gas feed and fuel, and the levelized cost is highly sensitive to the price of natural gas and relatively insensitive to the CAPEX. Revenues from syngas could have a significant impact on the net cost of electricity (COE), depending on the cost of natural gas and the selling price of syngas, estimated at $36 per MWh if the syngas were sold at $195 per ton. Following DOE NETL’s guidance, a lifecycle analysis (LCA) was conducted to compare with SMR. The functional unit for the basis of comparison was defined as 1kg carbon monoxide in the product stream. The global warming potential (GWP) of our process was found to be 40% lower than the state-of-the-art SMR process. The sensitivity analysis confirms the emissions are most sensitive to the natural gas fuel requirements to deliver heat to the process.

01 COAL, LIGNITE, AND PEAT↗