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At least 253 records · Page 14

Salt-Mediated Coarsening in Conversion-Reaction-Synthesized Nanoporous Metals and Nanocomposites Resolved through In Situ Synchrotron Diffraction Studies

High-energy synchrotron X-rays were used to probe the structural and microstructural evolution in Fe, Co, and Cu nanoporous metals (NPMs) and metal/salt nanocomposites (NCs) produced by recently developed conversion reaction synthesis (CRS) methods. Microstructure analysis of as-synthesized samples via whole pattern fitting showed that the NPMs exhibit domain sizes that increase as Co < Fe < Cu, with both Fe and Co having crystallite sizes below 3.0 nm. The as-synthesized metal/salt NCs had similar metal sizes, and additionally, the salt in the composite had unusually large lattice microstrain whose origin is attributed to chemical substitution of metal ions into the salt (e.g., Li $1–3x$ Fe $x$ Cl for Fe 3+ ). When thermal annealing is used to modify crystallite size, pore collapse often occurs in NPMs but NCs can be effectively tuned without this problem. While the NC coarsening occurs slowly at low temperatures, it was found that there is a drastic acceleration of the reaction rate at a specific onset temperature that results in the crystallite size increasing by an order of magnitude in about a minute. Curiously, there was no evidence in the diffraction data for salt melting at this onset temperature. However, there was a sharp reduction in the salt chemical lattice strain at the onset temperature, indicating that rapid metal coarsening is facilitated by the salt. Importantly, this behavior indicates an unexpectedly coupled reaction mechanism by which the metal ions needed for grain growth are supplied by the salt in a rate-limiting fashion.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Spark plasma sintering (SPS) densified U 3 Si 2 pellets: Microstructure control and enhanced mechanical and oxidation properties

Dense U 3 Si 2 pellets with controlled grain structure and enhanced thermal-mechanical and oxidation properties are synthesized with spark plasma sintering (SPS). Microstructure and phase composition of the SPS densified pellets are characterized systematically using SEM, EDS, and XRD. Thermal-mechanical properties and oxidation behavior of the sintered silicide fuel pellets are analyzed by laser flash, indentation, and dynamic thermogravimetric analysis. Dense U 3 Si 2 pellets are consolidated by combining high energy ball milling and rapid sintering by SPS, and the microstructure structures are controlled from micron-sized (~5.7 μm grain size) for conventional silicide to a nanocrystalline matrix with an average grain size of ~280 nm. A dominant phase of distorted U 3 Si 2 was identified with lattice expansion due to residual thermal stress upon SPS consolidation and rapid cooling processes. Both micron-sized and nano-sized pellets show exceptional thermal transport properties, consistent with monolithic silicides reported in literature. The SPS-densified pellets possess simultaneously high hardness and fracture toughness. The SPS-densified silicide pellets also demonstrate exceptional oxidation performance with extended onset oxidation temperature above 500 °C and reduced oxidation kinetics, particularly for nano-sized pellets. A strong strain effect was proposed in which compressive stress in nano-sized pellets enhances the oxidation resistance of silicide fuels, as evidenced by the degradation of oxidation performance upon strain relaxation by isothermal annealing. The correlation among the sintering process – microstructure control – physical properties and fuel behavior is established. A new concept of strain engineering is proposed further properties optimization, enabling the development of potential oxidation and corrosion-resistant silicides with extended performance, the key technological challenge of U 3 Si 2 as the leading concept of accident tolerant fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Manufacturing Li 2 TiO 3 -based tritium breeder materials by volume-controlled spark plasma sintering with an optimized microstructure

Multifunctional ceramic breeder materials are highly desirable for the deuterium-tritium fusion to achieve high efficiency in breeding tritium through neutron irradiation of lithium-containing blankets. Li 2 TiO 3 displays unique attributes as a potential ceramic breeder material. An optimized microstructure with three-dimensional interconnected pore structure is required for rapid transport of the tritium for effective fuel cycle, which however enviably results in the degradation of the thermal-mechanical properties of the breeding materials. In this work, nanocrystalline porous Li 2 TiO 3 ceramic pellets with controlled porosities of 14% and 20% are manufactured by volume-controlled spark plasma sintering. An optimized 3D interconnected pore structure is achieved consisting of both micro-sized pores and nano-sized pores embedded in nanocrystalline matrix, which could be beneficial to facilitate easy removal of bred T and He. Further, the 3D interconnected porous structure is well maintained upon isothermal annealing of the SPS-fabricated pellets at relevant operation temperature of the solid breeding materials. Single-phasic porous pellets also display enhanced thermal-mechanical properties, superior to current state-of-the-art materials which establish their potential as a promising tritium breeder material for nuclear fusion applications.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Evolution of microstructure and strength of a high entropy alloy undergoing the strain-induced martensitic transformation

In a recent work, we have reported outstanding strength and work hardening exhibited by a metastable high entropy alloy (HEA), Fe 42 Mn 28 Co 10 Cr 15 Si 5 (in at. %), undergoing the strain-induced martensitic transformation from metastable gamma austenite (γ) to stable epsilon martensite (ε). However, the alloy exhibited poor ductility, which was attributed to the presence of the brittle sigma (σ) phase in its microstructure. The present work reports the evolution of microstructure, strength, and ductility of a similar HEA, Fe 38.5 Mn 20 Co 20 Cr 15 Si 5 Cu 1.5 (in at. %), designed to suppress the formation of σ phase. A cast and then rolled plate of the alloy was processed into four conditions by annealing for 10 and 30 min at 1100 °C and by friction stir processing (FSP) at tool rotation rates of 150 and 400 revolutions per minute (RPM) to facilitate detailed examinations of variable initial grain structures. Neutron diffraction and electron microscopy were employed to characterize the microstructure and texture evolution. The initial materials had variable grain size but nearly 100% γ structure. Diffusionless strain induced γ→ε phase transformation took place under compression with higher rate initially and slower rate at the later stages of deformation, independent on the initial grain size. The transformation facilitated part of plastic strain accommodation and rapid strain hardening owing to a transformation-induced dynamic Hall-Petch-type barrier effect, increase in dislocation density, and texture. Here, the peak strength of nearly 2 GPa was achieved under compression using the structure created by double pass FSP (150 RPM followed by 150 RPM). Remarkably, the tensile elongation exhibited by the alloy was nearly 20% with fracture surfaces featuring a combination of ductile dimples and cleavage.

36 MATERIALS SCIENCE↗

Correlative electron and ion beam analysis of the electrochemical performances of LiV 3 O 8 cathode films as a function of microstructures

Degradation mechanisms in LiV 3 O 8 cathode films (~500 nm) with different initial microstructures i.e., globular nanocrystals in amorphous matrix and needle-like nanocrystals, synthesized by annealing the cathodes at 150 °C and 300 °C for 6 h are studied by Transmission Electron Microscopy (TEM) and Auger Electron Spectroscopy (AES). In addition, a unique in-situ combination of TEM and Secondary Ion Mass Spectrometry (SIMS) imaging techniques, namely Parallel Ion and Electron beam Spectrometry (PIES) is carried out to measure the 3D distribution of V and Li with nanoscale resolution. These characterization studies focus on correlating the pre- and post-cycling microstructure to observed electrochemical performance. The LiV 3 O 8 cathode film with needle-like nanocrystals (300 °C) shows a higher initial capacity but it degrades rapidly compared to the film with globular nanocrystals embedded in amorphous matrix (150 °C). We observed that LiV 3 O 8 films with needle-like nanocrystals are more susceptible to cathode decohesion and vanadium dissolution than the films with globular nanocrystals embedded in amorphous matrix, explaining the differences in their electrochemical performance. The findings from this study have relevance to the development of thin film electrode microstructures for high capacity and cyclic stability.

25 ENERGY STORAGE↗

GdWN 3 is a nitride perovskite

Nitride perovskites ABN3 are an emerging and highly underexplored class of materials that are of interest due to their intriguing calculated ferroelectric, optoelectronic, and other functional properties. Incorporating novel A-site cations is one strategy to tune and expand such properties; for example, Gd 3+ is compelling due to its large magnetic moment, potentially leading to multiferroic behavior. However, the theoretically predicted ground state of GdWN 3 was a non-perovskite monoclinic structure. Here, we experimentally show that GdWN 3-y crystallizes in a perovskite structure. High-throughput combinatorial sputtering with activated nitrogen is employed to synthesize thin films of Gd 2-x W x N 3-y O y with oxygen content y < 0.05. Ex situ annealing crystallizes a polycrystalline perovskite phase in a narrow composition window near x = 1. LeBail fits of synchrotron grazing incidence wide angle x-ray scattering data are consistent with a perovskite ground-state structure. Refined density functional theory calculations that included antiferromagnetic configurations confirm that the ground-state structure of GdWN 3 is a distorted Pnma perovskite with antiferromagnetic ordering, in contrast to prior predictions. Initial property measurements find that GdWN 3-y is paramagnetic down to T = 2 K with antiferromagnetic correlations and that the absorption onset depends on cation stoichiometry. This work provides an important path toward both the rapid expansion of the emerging family of nitride perovskites and understanding their potential multiferroic properties.

14 SOLAR ENERGY↗

Containerless drop tube solidification and grain refinement of NiAl3

The possibility of undercooling Ni-Al alloys below the liquidus in order to produce a single phase peritectic structure by containerless drop tube solidification was studied. Containerless process is a technique for both high purity contamination free studies as well as for investigating the undercooling and rapid solidification of alloys by suppression of heterogeneous nucleation on container walls. In order to achieve large undercoolings one must avoid heterogeneous nucleation of crystallization. It was shown that the Marshall Space Flight Center drop tubes ae unique facilities for containerless solidification experiments and large undercoolings are possible with some alloys. The original goal of undercooling the liquid metal well below the liquidus to the peritectic temperature during containerless free to form primarily NiAl3 was achieved. The microstructures were interesting from another point of view. The microstructure from small diameter samples is greatly refined. Small dendrite arm spacings such as these could greatly facilitate the annealing and solid state transformation of the alloy to nearly 10% NiAl3 by reducing the distance over which diffusion needs to occur. This could minimize annealing time and might make it economically feasible to produce NiAl3 alloy.

Ethridge, E. C.↗

Tuning Strong Metal–Support Interaction Kinetics on Pt-Loaded TiO 2 (110) by Choosing the Pressure: A Combined Ultrahigh Vacuum/Near-Ambient Pressure XPS Study

Pt catalyst particles on reducible oxide supports often change their activity significantly at elevated temperatures due to the strong metal–support interaction (SMSI), which induces the formation of an encapsulation layer around the noble metal particles. However, the impact of oxidizing and reducing treatments at elevated pressures on this encapsulation layer remains controversial, partly due to the “pressure gap” between surface science studies and applied catalysis. In the present work, we employ synchrotron-based near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS) to study the effect of O 2 and H 2 on the SMSI-state of well-defined Pt/TiO 2 (110) catalysts at pressures of up to 0.1 Torr. Further, by tuning the O 2 pressure, we can either selectively oxidize the TiO 2 support or both the support and the Pt particles. Catalyzed by metallic Pt, the encapsulating oxide overlayer grows rapidly in 1 × 10 –5 Torr O 2 , but orders of magnitude less effectively at higher O 2 pressures, where Pt is in an oxidic state. While the oxidation/reduction of Pt particles is reversible, they remain embedded in the support once encapsulation has occurred.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High-throughput investigation of crystal-to-glass transformation of Ti–Ni–Cu ternary alloy

A high-throughput investigation of metallic glass formation via solid-state reaction was reported in this paper. Combinatorial multilayered thin-film chips covering the entire Ti-Ni-Cu ternary system were prepared using ion beam sputtering technique. Microbeam synchrotron X-ray diffraction (XRD) and X-ray fluorescence (XRF) measurements were conducted, with 1,325 data points collected from each chip, to map out the composition and the phase constitution before and after annealing at 373 K for 110 hours. The composition dependence of the crystal-to-glass transition by solid-state reaction was surveyed using this approach. The resulting composition-phase map is consistent with previously reported results. Time-of-flight secondary ion mass spectroscopy (ToF-SIMS) was performed on the representative compositions to determine the inter-diffusion between layers, the result shows that the diffusion of Ti is the key factor for the crystal-to-glass transition. In addition, both layer thickness and layer sequence play important roles as well. This work demonstrates that combinatorial chip technique is an efficient way for systematic and rapid study of crystal-to-glass transition for multi-component alloy systems.

36 MATERIALS SCIENCE↗

High-Throughput Automated Exploration of Phase Growth Behaviors in Quasi-2D Formamidinium Metal Halide Perovskites

Quasi-2D metal halide perovskites (MHPs) are an emerging material platform for sustainable functional optoelectronics, but the uncontrollable, broad phase distribution remains a critical challenge for applications. Nevertheless, the basic principles for controlling phases in quasi-2D MHPs remain poorly understood, due to the rapid crystallization kinetics during the conventional thin-film fabrication process. In this work, a high-throughput automated synthesis-characterization-analysis workflow is implemented to accelerate material exploration in formamidinium (FA)-based quasi-2D MHP compositional space, revealing the early-stage phase growth behaviors fundamentally determining the phase distributions. Upon comprehensive exploration with varying synthesis conditions including 2D:3D composition ratios, antisolvent injection rates, and temperatures in an automated synthesis-characterization platform, it is observed that the prominent n = 2 2D phase restricts the growth kinetics of 3D-like phases—α-FAPbI 3 MHPs with spacer-coordinated surface—across the MHP compositions. Thermal annealing is a critical step for proper phase growth, although it can lead to the emergence of unwanted local PbI 2 crystallites. Additionally, fundamental insights into the precursor chemistry associated with spacer-solvent interaction determining the quasi-2D MHP morphologies and microstructures are demonstrated. The high-throughput study provides comprehensive insights into the fundamental principles in quasi-2D MHP phase control, enabling new control of the functionalities in complex materials systems for sustainable device applications.

2D perovskites↗

Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED

The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.

Source record↗

Preliminary Low Temperature Electron Irradiation of Triple Junction Solar Cells

For many years extending solar power missions far from the sun has been a challenge not only due to the rapid falloff in solar intensity (intensity varies as inverse square of solar distance) but also because some of the solar cells in an array may exhibit a LILT (low intensity low temperature) degradation that reduces array performance. Recent LILT tests performed on commercial triple junction solar cells have shown that high performance can be obtained at solar distances as great as approx. 5 AU1. As a result, their use for missions going far from the sun has become very attractive. One additional question that remains is whether the radiation damage experienced by solar cells under low temperature conditions will be more severe than when measured during room temperature radiation tests where thermal annealing may take place. This is especially pertinent to missions such as the New Frontiers mission Juno, which will experience cell irradiation from the trapped electron environment at Jupiter. Recent testing2 has shown that low temperature proton irradiation (10 MeV) produces cell degradation results similar to room temperature irradiations and that thermal annealing does not play a factor. Although it is suggestive to propose the same would be observed for low temperature electron irradiations, this has not been verified. JPL has routinely performed radiation testing on commercial solar cells and has also performed LILT testing to characterize cell performance under far sun operating conditions. This research activity was intended to combine the features of both capabilities to investigate the possibility of any room temperature annealing that might influence the measured radiation damage. Although it was not possible to maintain the test cells at a constant low temperature between irradiation and electrical measurements, it was possible to obtain measurements with the cell temperature kept well below room temperature. A fluence of 1E15 1MeV electrons was selected as representative of a moderately high dose that might be expected for a solar powered mission. Fluences much greater than this would require large increases in array area and mass, compromising the ability of PV to compete with non-solar alternatives.

Stella, Paul M.↗

Elevated-Temperature Deformation Properties of a HfC Modified Ti-48Al-2Mn-2Nb Matrix Particulate Composite

Rapid solidification techniques in combination with HIPing have been used to produce Ti-48Al-2Mn-2Nb and a Ti-48Al-2Mn-2Nb+15 wt% HfC composite. While the composite does contain several second phases within the gamma + alpha(sub 2) matrix, none was identified to be HfC. The elevated-temperature properties were determined by constant velocity compression and constant load tensile testing in air between 1000 and 1173 K. Such testing indicated that the elevated temperature strengths of the HfC-modified aluminide was superior to those of the unreinforced matrix with the best 1100 K temperature slow strain rate properties for both materials being achieved after high-temperature annealing prior to testing. Examination of the microstructures after deformation in combination with the measured stress exponents and activation energies suggest that creep resistance of the HfC-modified form is due to solid-solution strengthening from carbon and hafnium rather than the presence of second phases.

Whittenberger, J. D.↗

Effect of Heat Treatment on Microstructure and Mechanical Property of 316L Stainless Steel Produced by Laser Powder Bed Fusion

The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.

36 MATERIALS SCIENCE↗

On optical properties and scintillation performance of emerging Ga 2 O 3 : Crystal growth, emission mechanisms and doping strategies

As an emerging ultra-wide bandgap compound semiconductor, Ga 2 O 3 has attracted rapidly growing interest due to its unique physical properties for harsh condition applications. Compared to Ga 2 O 3 ’s electrical-characteristic based uses, such as power electronics, photodetectors and solar cells, a much less explored area for Ga 2 O 3 is its promising optical properties and its related scintillation capabilities. Undoped Ga 2 O 3 is a strong scintillator with excellent scintillation characteristics such as fast decay constants and encouraging light yield which is comparable to that of the classic Bi 4 Ge 3 O 12 (BGO) scintillator. The scintillation capability of Ga 2 O 3 can be precisely tuned via a series of approaches including systematic crystal growth control, post-growth annealing, targeted doping, and optimization of operation temperature. Here we summarize exciting progress of Ga 2 O 3 scintillators which have been pursued over the past few years. Our efforts cover a series of growth techniques of Ga 2 O 3 materials as well as discussion of emission mechanisms. Here we dedicate a targeted portion toward the doping strategies to improve the performance of Ga 2 O 3 . A detailed analysis is provided to compare the impact of different dopants. Through these efforts, we hope to provide useful perspectives to help accelerate the development of high performance Ga 2 O 3 scintillators.

36 MATERIALS SCIENCE↗

Fuel-Cladding Eutectic Study of Legacy Fast Flux Test Facility (FFTF) MFF HT9/U-10Zr Metallic Fuel

This report presents the first systematic investigation of fuel-cladding eutectic interaction (FCEI) in irradiated HT9/U-10Zr metallic fuel from the Fast Flux Test Facility (FFTF) Materials Fuels Form (MFF) program, using differential scanning calorimetry (DSC) coupled with scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Two irradiated fuel cross-sections, MNT07H (9.5 at% burnup, x/L = 0.78) and MNT08H (7.0 at% burnup, x/L = 0.93), were subjected to three successive isothermal annealing rounds (R1–R3) at 820°C for 20 minutes each, yielding a cumulative transient duration of one hour. This study directly addresses a recognized gap in the existing FCEI database, which previously lacked irradiated HT9/U-10Zr data at burnup levels above 8 at%. Two principal findings emerge from the study. First, for both samples, FCEI remained spatially confined within the pre-existing fuel-cladding chemical interaction (FCCI) zone boundaries after R3, with no measurable eutectic penetration into unaffected cladding beyond the original FCCI layer. This self-limiting behavior is consistent with historical Fuel Behavior Test Apparatus (FBTA) results and is attributed to the near-eutectic phase composition of the FCCI zone, which rapidly absorb the available eutectic-forming constituents and then stall penetration once the FCCI zone is consumed. A comparison with unirradiated surrogate data further supports this mechanism: whereas a U–34 at.% Fe sample would be expected to show ~176 µm of iron penetration under comparable conditions, the irradiated samples exhibited only ~20 µm, a discrepancy attributed to irradiation-induced interfacial porosity and pre-existing FCCI composition gradients. Second, for MNT08H, FCEI was observed exclusively on the half of the cladding circumference where pre-existing steady-state FCCI was present, with no detectable FCEI on the opposite half. Three hypotheses are proposed to explain this asymmetry: the inhibiting role of a zirconium-rich rind at the fuel-cladding interface; the chemical sequestration of iron by redistributed zirconium within the fuel matrix; and the persistence of fuel-cladding gaps on the FCEI-free half that preclude direct contact. All three hypotheses require further experimental investigation. The results extend the empirical FCEI database into higher-burnup territory and demonstrate the viability of DSC-based testing as a substitute for the no-longer-available FBTA apparatus. Future work will include additional cross-section testing, compilation of the full FCEI dataset, model evaluation, and DSC testing of ternary fuel compositions to broaden the experimental basis for safety assessment of sodium-cooled fast reactor systems.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Interfacial Connections between Organic Perovskite/n + Silicon/Catalyst that Allow Integration of Solar Cell and Catalyst for Hydrogen Evolution from Water

Abstract The rapidly increasing solar conversion efficiency (PCE) of hybrid organic–inorganic perovskite (HOIP) thin‐film semiconductors has triggered interest in their use for direct solar‐driven water splitting to produce hydrogen. However, application of these low‐cost, electronic‐structure‐tunable HOIP tandem photoabsorbers has been hindered by the instability of the photovoltaic‐catalyst‐electrolyte (PV+E) interfaces. Here, photolytic water splitting is demonstrated using an integrated configuration consisting of an HOIP/n + silicon single junction photoabsorber and a platinum (Pt) thin film catalyst. An extended electrochemical (EC) lifetime in alkaline media is achieved using titanium nitride on both sides of the Si support to eliminate formation of insulating silicon oxide, and as an effective diffusion barrier to allow high‐temperature annealing of the catalyst/TiO 2 ‐protected‐n + silicon interface necessary to retard electrolytic corrosion. Halide composition is examined in the (FA 1‐x Cs x )PbI 3 system with a bandgap suitable for tandem operation. A fill factor of 72.5% is achieved using a Spiro‐OMeTAD‐hole‐transport‐layer (HTL)‐based HOIP/n + Si solar cell, and a high photocurrent density of −15.9 mA cm −2 (at 0 V vs reversible hydrogen electrode) is attained for the HOIP/n + Si/Pt photocathode in 1 m NaOH under simulated 1‐sun illumination. While this thin‐film design creates stable interfaces, the intrinsic photo‐ and electro‐degradation of the HOIP photoabsorber remains the main obstacle for future HOIP/Si tandem PEC devices.

08 HYDROGEN↗

Influence of Disorder on the Electronic Properties and Magnetotransport of Ti 3 C 2 T x Single-Flake Devices

The exploration of MXenes for electronic applications is a rapidly growing field in materials science. However, most research has focused on MXene films, with only a limited number of studies addressing the characterization of single-flake devices. In this work, we investigate the electronic and magnetotransport properties of Ti 3 C 2 T x single-flake devices, exploring the influence of structural defectivity on their transport mechanisms. We show that negative magnetoresistance present at low temperatures in single flake samples arises from weak localization, which we analyze to extract the phase coherence length of single-layer and multi-layer flakes. The study of magnetoresistance for this metallic MXene shows that the material exhibits quantum transport phenomena when intrinsic electronic behavior dominates. Moreover, by increasing the defect density via thermal annealing in ultrahigh vacuum, we uncover and characterize the metal-to-disordered metal transition in Ti 3 C 2 T x , shedding light on new properties and enriching fundamental knowledge about MXenes.

MXenes↗